SCIENTIFIC ABSTRACT SHCHEGOLEVA, R.P. - SHCHEGOLEVA, V.I.
Document Type:
Collection:
Document Number (FOIA) /ESDN (CREST):
CIA-RDP86-00513R001548810011-2
Release Decision:
RIF
Original Classification:
S
Document Page Count:
100
Document Creation Date:
November 2, 2016
Document Release Date:
March 14, 2001
Sequence Number:
11
Case Number:
Publication Date:
December 31, 1967
Content Type:
SCIENTIFIC ABSTRACT
File:
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Body:
s/129/65/000/002/Oo6/ol4
Dilatometric studies .... l 9 5 / E13 Ull 3
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Card 4/4
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L - 112�M3 LIWP~q)/EWT(m)/BIX5--AFFTG/ASD--JD, -- - - -- - - -- - - -- -i
SICK M. AP300195 S/0226/63/000/003/0088/0098
5_&
AMO.R., Borok, B. Ae.; Golifbeva, L. ST; Shchegoleva, R. Ruch 'yeva, X. A
TITLE: Mechanical properties and microstructure of sintered titsniun alloys
SOURCE: Foroshkoraya, metallurgiya, no- 3, 1963, 88-98
TOPIC TAGS: sintered titanium alloys, mechanical properties, m1crostructurc,
grain size., alloying element effect, Fe, Min, Cr, Mo, Al, V~, W, Ta., Nb, Cla,,
Zr' Co Ti-Al-V alloy, Ti-Al-V-Mo alloy, coreduction, oxide
ABSTRACT: Several series of binary and ternary alloys of Ti with Al, Fe, bin,
Cr, Mo. W., V Ta, Nb., Cu,, Zr.. and Co were sintered frcm cam-ercial-grade
(99.17~ puree Ti powder and parders of gg.&,,. pure Fe, 99.5% pure mu, 99.69%
.:Duxe Cr, 99-54% pure Ni, 99.4 pure Co, electrolytic Cu, 99. 8% -pure W, 99.65%
pvxe Mo, 99.62F,16' pure V, 98.6~ pure 14b, and 98.6% pure Ta. The Ti-Al alloys
and the second series of Ti-V alloys were prepa-red by coreduction of oxide
powders with calcium hydride. Sintered specimens had a. coarse, acicular micro-
-structure, macrograins about 1 = in diameter, and a density of 97-99% of the.
theoretical. The results of mechanical tests (see Figs. 1 and 2 of Enclosux&)~
s1how that all the.alloying elements investigated increase the tensile strengt4_*
Card
7~ (2155)
L 11288-63
AccEssioN im: Anoo1956
and decrease the ductility of sintered Ti alloys. Cnly in Ti-V 8-cloys Pro-
duced by coreduction. of oxides does ductility increase with increasing V
content. These alloys generally are more ductile than commercial titanium.
The strong 0-phase stabilizersY Fem, M, and Cr, which promote autectoid trans-
formation with the formation of intermetallic acmpounds,, produce the highest
increase in tensile strength and decrease in ductility of sintered Til alloys.
The Ti-Fe, Ti-Ma, Ti-Cr, and Ti-If alloys containing 2-10% of the following ele-
ment have a metastable a + 13 structure with the amount of "the P-phase increas-
ing with higher alloying; the a-phase has an acicular WidmanstAtten structure.
AluminumY an a-phase stabilizer, appreciably increases the strength of sintered
Ti-Al alloys without an extensive decrease in ductility. Vie Ti-V and Ti-Yio
alloys have comparatively high tensile strength and ductility. In general, V,
Al. and Mo were found to be the best a"oying elements for sintered binary Ti
alloys. Additional investigation of sinterea Ti-Al-V alloys (produced by core-
duction of the oxides) shoved the Ti + 3% Al + Yp V alloy to have the best ccm-
bination of mechanical properties: tensile strength of 774-2 Mn/W? (meganewton
per square meter, 1 Ma/M 2 = 0.1 kg/mm?], elongation 15%, redilction. of area 26,,,.',,
and notch toughness 25.4 joule per cm2 (I joule/cmP 0.1 m-]:~g/cmPl. An addi-
tion of 2% Mo to this alloy increases its tensile strength to 857-5 14n/M:R without
:Lowering ductility. These two alloys are recoomended for manufacturing parts by
Card 2/~
ACCESSION Nki AP4040471 S/0226/64/000/003/0050/0063
'AUTHOR: *Borok, B. A.; Shchegoleva, R. P.; Golub.ova, Lo So;
Teplenko, V. C.; Reutova,-rif- P.,;.Ruch'yeva, No A,
TITLE: Properties and microstructure of sintered Khl8Nl5 stainloss
steel mado by joint reduction method
'SOURCEs Poroshkovaya metallurgiya, no. 3 (21), 1964, 50-63
.TOPIC TAGS: stainless steel, sintered stainless steel, carbonyl
iron, sintered steel property, steel corrosion resistance, sintered
!steel structure
Investigations have been made of the properties of
:sintered Khl8N15 chromium-nickel-stainless steel made from powder
iproduced by the joint reduction of chromium and nickel oxides
mixed with iron powders (Process A) and of steel made from mechani-
ically mixed powders of carbonyl iron, reduced chromium, and electro-
ilytic nickel (Process B). It was found-that the density of compacts
'A was lower that that of Do but the latter had a very low compression
;strenath. Adequate fluidity of powders and strength of compacts
Lq~rd
ACCESSION HR: AP4040471
make powder A a very suitable material for rolling porous strips
and sheets in continuous rolling mills. Compacts B sinter more easily
than compacts A, but they are much more- susceptible to oxidation
during the sintering. Compacts A, sintered at 1350C for 10 hr; had
a density of 96-97% (compared to 71-85% for compacts B), tensile
.strength 47.8-53.5 dan/mm2 , elongation 29.2-43.4% and impact
toughness(unnotched specimens)19.8-29 kgm/cm2, Sintered KhIBN15
steel has an austenitic. structure with a low content of finely
.dispersed carbides. In the annealed state the steel has a high
corrosion resi'stance; its corrosion rate in boiling 65Z nitric acid
Js 0.1 g/M2- hr compared to 0.2 g/m2- hr for conventionally made
:X18H15. This is explained by a low content of impurities in powder
Orig. art. has.* 8 tables and 9 figures.
.ASSOCIATIONt Tsentral'nyky nauchno-inaledovatel'skiy institut chernoy
metallurgLi (Central Scientific Research Institute of Ferrous
:Metallurgy)
G?rd 2 /3
-66 L
.vp(e
L 2847
v.PdIJ D/WB
ACCESSION NR: AT5022891 UR/2776/65/000/043/0081/0098
AUTHOR: ShcheRoleva, R. P.; geutova, N. P.; Colubeva, L. S.; FaILAvakaya, V. L.!
..-Kazanakaya.' 1:.
TITLE: Powdered-metal stainlessehrome and chrome-nickpi _Lta"_ d
/SOURCE: Moscow. Tsentral'nYY nauchno-iseledovatel'skiy instituLlhIrno m
ak~*_'tallurgii. Sbornik trudov, no. 43, 1965. Poroshkovaya metallurgiya (Powder metal-
lurgy), 817~98
TOPIC TAGS: powder metallurgy, stainless steel, chromium steel, nickel steel,
corrosion resistance
ABSTRACT: It is shown that the powders of stainless chrome and chrome-nickel
steels in the ferritic, austenitic, and martensitic-ausbenitic classes, prepared
-
by the method of the combined reduction of metal oxideAy means of CaR are
suitable for the industrial fabrication of porous and compact sheets an
by the direct method of powder rolling. The flowsheet of production of these
powders has the following sequence: raw materials -- iron powder (carbonyl and
other types of Fe), chromium oxide (Cr203), nickel (electrolytic, carbonyl)
I Card 1/3
_h ~847-66__
ACCESSION NR: AT5022891
powder or NiO, Ni 0
2 3, calcium hydride (CaH2); charge blending (2.5 hr); reduction
iat 1175*C for 6-8 hr, Cr203 + 3CaH2 - 2Cr + 3CaO + 3H2; crushing of sinter;
slaking with H20 and pulverization; hydrocyclone treatment of pulp; leaching --
Ca(OH)2 + 2HCl - CaCl2 + 2H20; washing to remove CaCl2; centrifuging; vacuum
drying, 60-70*C. Sintered stainless steels display high physical properties,
which warrants recommending them for the fabrication of the elements and devices
2
performing in aggressive media. When pressed under a pressure of 10 t/cm and
subjected to deformation and heat treatment, powdered-metal stainless steels are
not inferior to steels produced by the smelting method a regards their physical
properties and corrosion resistance. Thus, for example, corrosion tests of
Khl8NI5 stainless austenite steel in a 65% solution of boiling HN03 demonstrated
,~the high corrosion strength of this steel, not inferior*to that of deformed cast
steel (corrosion rate 0.1-0.16 g/m2-hr). Evidently these good qualities of pow-
dered-metal stainless steels are attributable to the low content of impurities
in the powders prepared by the combined oxide reduction method. Orig. art. has:
10 figures, 9 tables.
ASSOCIATION; none
Card 2/3
! L 2847-66
i ACCESSION NR:
I
i
SUBMITTED: C
q
NO
I
[__V k
-Card
11
? -
'AT5022891
i
0 !
I
L 2679-95 E'4'P(e)/E;','T(m)/4VIA(d)/EWP(t)/EWP(k)/EVIP(z)/F-IVP(b)-.---IJP(c) MJWI-
ACCESSION MR: AT5022892 JD/HW UR/2776/65/000/043/0099/0108
AUTROR: Solov,yeva, Z. V.; Golubeva,_ L. S.; Shcheizoleva, R. J~; Rqqh_!jMiA_fi_-
TITLE: Investigation of the properties. and production conditions of nichrome
powder
SOURCE: -Moscow. T6entral'nyy nauchno-isslgdovatel'gkiy inq#tZut cherngy
lurgiii"Sbornik trudov, no. 43, 1965. Foroshkovaya metallurgiya. (Powder metal-
lqrgy),,99-ln8
OPIC TAGS: nichrome alloy, powder alloy, nonmetallic inclusion, sintering,
solid solution, twinning, heat resistant allo resistivity
ABSTRACT: In view of the deviations observed in th tec:hnological,,/properties of
the products fabricated from the powder of Kh20N8 11 ichr ag_aj-1Qy1~repared by the
method of the combined reduction of metal oxides with CaH2 developed by the
Central Scientific Research Institute of Ferrous HetallmKiy,~4t~e authors per-
formed a thorough investigation of the parameters of the process. Gas analyses
and -.--'.1ographic examinations established that nichrome po-fders obtained at
Card
1j3
L 2679-66
ACCESSION NR: AT5022892
oxide-reduction temperatures of 900-1100*C (for 6 hr) contain a considerable
amount of non-metallic inclusions, associated with the higher content of oxygen.
This condition is corrected (the oxygen content is reduced to the required mini-
mum of 0.4% and the microstructure becomes homogeneous) by raising to 1175*C the
reduction temperature and performing reduction for 6-8 hr (6 hr for 219-mm dia-
meter retort and 8 hr for 273-mm diameter retort). However, while the powder pre-
pared at 1175*G for 6-8 hr displays the optimal compactibility, its sinterabilit
,is much lower than in powders prepared at lower reduction temperatures (900-
11000C), which evidently is attributable to the activizing effect cf oxygen as
well as to granulometric composition. Since, the oxygen content may not exceed
0.047., it appears that sinterability can be improved only by altering the granu-
lometric composition of the powder. This composition can be regulated within
broad limits by pulverizing the sinter (pulp) for 0.5, 1.0, 1.5, and 2 hr. To
evaluate its quality, the powdered-metal nichrome prepared on the basis of the
above improvements was subjected to heat treatment and cold working and tested
for physical properties. Specimens compacted under a pressure of 6.0-6.8 tons/cM2
arld sinLered at the maximum temperature (1375*C) were found to display the highesti
ultimate strength and plasticityj?Wir-e of 0.5-2.0 mm diameter7-fabricated from
sintared briquets displays, following its heat treatment (water quenching from
Cord 2/3
L 2619-66
ACCESSION NLR: AT5022892
870*C), physical properties as high as those of standard nichrome wire. Follow-
ing its sintering, as well as following its forging in the temperature range
1000-1200*C, the powdered-metal nichrome has the monophase structure of a nickel-
base solid solution with grain boundaries clearly revealed by etching. *:ol
its annealing at 800 or 900% the nichrome displays the typical structure of
nickel austenita; the grain orientation changes and a large number of tiins
appears. In addition to their high heat resistance and resistance to ox*.dation
at high temperttures, the products,fibricated from such nichrome powder display
a high resistivity (1.07-1.12 ohm-mm /m). Orig. art. has: 10 figures, 6 tables.
ASSOCIATION: none
SUBMITTED: 00 ENCL: 00 SUB CODE: M, is
NO REF SOV: 007 OTHER: 004
Card 31-
L 2680-66 E71T(M)/EViA (d)/EVjp1't)/.-WP(z)/EWP(b) M JVI/ J-D
ACCESSION NR: AT5022893 UR/2776/65/000/043JO109/0114
AUTHOR: Shchegoleva, R. P.i,Golubeva, L. S,; Ruch'yeva, N. A.; Poplavskaya, V. L.'
TITLE: Investigation of the mi:rostructure of alloy powders obtained by the
combined reduction method
SOURCE: 14oscow. Tsentral'nyy nauchno-issledovatel'skiy iistitut cheEaoy Re
"L
lurgii.44-~bornik trudov, no. 43, 1965. Poroshkovaya metallurgiya (Powder metal-
lurgy), 109-114
TOPIC TAGS: metal powder, alloy powder, nichrome alloy, grain structure
ABSTRACT: The process of the combined xtducCiori of metal powders and oxides by
means of CaH2 usually takes place in the solid phase, and then the gran-uTa-metric
composition of the resulting powder is chiefly determined by two factors: 1)
physical properties of raw materials; and 2) the process of agglomeration of the
metal particles (this process takes place in the solid phase for both fine- and
coarse-grained materials). Studies of a large number of industrial batches of the
powder of Kh20N80 nichrome established that distinct structural inhomogeneities
appear only when the technological regimes of production are.diaregarded. Such
Card 1/3
L 2680-66
ACCESSION NR: AT5022893
inhomogeneities are manifested in the form of the presence of a second phase al-
though no such phase was revealed by radiographic examination. A microscopic.
examination of the Sulin and Tula iron powders revealed, along with particles
having ferrite structure, isolated particles with ferrite + pearlite structure
conditioned by a higher content of C. Such nonuniformity of individual particles
as regards C content also persists in Khl8Nl5 steel. Particles with two-phase
structure have been observed in individual industrial batches of Fe-Al master
alloy powder which indicates violations of the technological r4 :Ci-ae _~_Daharge
blending, mixing, and reduction. The microstructural inhomogeneity of the powder
of Khl8Nl5 steel, conditioned by its content of alloy elements, is greater if the
camparatiAPely coarse-grained Sulin and Tula iron powders are used as part of the
raw materials. In this case an appreciable amount of a-phase is observed in the
microstructure of the large par!~cles. If, on the other hand, this steel, as
well as Kh20N80 nichrome alloy..Jis prepared from fine-grained raw materials, the
resulting powderVwill display some inhomogeneity with respect to the content
of alloy alements, owing to their extremely weak ferromagnetic properties. All
this, however, is no reason for rejecting the powders as defective, since, being
chiefly destined for processing into metallurgical products, they are subjected
to sintering, which involves complete homogenization of their composition.
2/3
Card
L 2680-66
ACCESSION NR: AT5022893
Orig. art. has: 5 figures.
ASSOCIATION: none
SUBMITTED: 00 ENCL: 00 SUB CODE: MM, IR
NO REF SOV: 007 OTM: 000
Card 3 /3
V Reaction o vin 4 ethers with amines A N* Kost A M Ove 30% quiraidine; PhNIH, and is6-BuOCH:CH3 gave*-,
-
I ra! Y gam.' d-=. t~~!he`i-.U.7.E~
jy1trkevich 34 -,a qtunwaine. Heating 21A g. p-MeCH,NHj. 10
g. I
,
jStatc Univ.). Zhur. UbsArUf A%R~.- BuOCH: CH., and 0.5 g. p-'MeC.H.NH..HCl in sealed tithe
t7him If S.S. R. 25, 907-10(1955XEngf, tran3lation);
Ven 20 hT3. at 100* gave 714% crude 2,6-dimethylquinoline, or
.
13622e~Syntheses of 2-methylquinolines from
C-A. 48
Cf 51% pure product, b, 106-7% tn. 59.5". purification with
'
.
,
vinyl ethirs and amines are described. To 9.3 g. PhNHI AcIO instead of steam dis tn. gave 54170 )idd, Dioxane
and 0.2 g. PhIxTH3.HCI was added dropwist at,95-100' 5 g. tends to raise the yield; the use of EtGCII- CHI gave a 36%
BuOCH: CHt and the mixt. heated gradually tct 130* over 4 yield. , Heating 21.4 g. o-%IeCJ-LNLH,,-l0 g. BuOCH.CH,.
firs. Distn. gave 2.7 g. quinaldine, b4 84-90* (picrate, m. and 0.5 g. o-MeCjH,NH~-HCI in 50 ml- dioxane 25 hrs. at
contg. traces of PhUH2. The same 3ield resulted
190-1*)
th-
reflux gave 66% 2,8-ditnethylquinoliue; purification W:
,
after25 days in sealed tube at room temp. Wlie--ia trace of. PhSC~Cl gave 44% pure product. white the use of Ac2O gave
*
BzzOp was used instead of PhNift-HO, the yield.-vas 34%; ). ToL2.3
58%;ptLrepruduct,b&103-4*(picrdtem.180-1
Bl,',.Et,O catalyst gave 30% yield. When 18.3 g. PhNHs, g. P4.lcOC$HjNH3, 0.5g. of its HCI salt, and 50 ml. diox-
-10 g. BuOCH:CH*, 0.5 g. PhNH3.HCI, and 40 mt. xylene ane w4sadded slowly at rellux over 2 firs. 10 g. BuOCH:CH2.
were heated 25 Ins. on a steam bath. then acidified, steam and the mirt. refluxed 16-18 hr3. to 1P ve 15% 2-m'~thyl-6-
.
to remove the solvent and BuOH, andthe residuemade,
distd the yield
methoxyqinoline, bs 120-~3% to. 67 ; at go
I
'
.
1k. and steam distd. spin, there was obtabiedO% quinal-
~ .
reaction took place.
drooped to 7%; without dioxame no
t 100*
s
d
ft
25 h
29%
H
NH
i
ld
l
2
C
~cation is made with AcsO, the yit!ld rises W
rpur
d if Ih -
r
e
a
er
. a
,
e
Simdar
o
t y
T
y
*
r ur_fi Dioxane-.
717.. , _,on with ZnCJt gives 33% yield.
), if an
-Imethy1m5,64--maquinoline, in. (p*rale, m. 221
Lve the same yield. but without 0t
i.,ea of ,I, ge he s
_.e
NM and I~tOCR: CH2
ches only 3350'.
quirnolar pr ts is used- -a 2:1 molar ratio:
oportion of reactan
i
ld
R
7
fl
i
ii
- gave
e
.
e
ttx
.K 10.9 g. o-
% y
.Ncal.off. 20 9.
BuOClf.CH,, 50 mi. dioxane, and 0.5 g. PhTNH2.HCl 20
firs. gave 10% 8-Adroxyqzanaldine, m. 700 (crude)
ft
bli
ti
Mi
i
(
6
er su
a
ma
on
x
ng 9.3 g. PhNHI, 10 g. B
CHe. 8.9 jr. nvruvir acid- 40 mL nhs M014- qnd njj
2 J
Usad-ltv;..
41th fori xild ad
t-Z
a juid L.
041
CA,
IOAAA
q__
-'Reduction with formic, acid and Its derivatives. III.
R,
synthesin of substitutod A. N. Kost,_
S I
~~7TM
.&olga and L. G. Who (State W
T. A. Shc~e
_V4 'TV.:
97 lain
Y
j,
J.W11e1Kh$m.25,2R -U(I 66); --A
-Reactions of 53 g. CH,,.CHCN and 200 g. AcCtl,COrt'
.with EtO-'4a in FtOH in 48 hrs. gave 5013'0 -y-carbrthoxy4-
ax0capranfirile, b%l43-4*,nV 1.44621,which refluxed withaq.
K&CO& 3.5 hrs. gave 70170 5-ox"apronitrile, bt, 108-9*, OU
1.44D3. This (10 g,) and 31 g. IICOsNa refluxed %vith 2.1 g.
100% 11M11, cooled, and dild., then treated with excess
40% NaOH gave M% Z-rncthyl-6-piperidene, m. 8.5% which
refluxed 5 hts. with coned. HCJ gave 6-amino proic acid-
Ca
110, m. 146-7*. A 24-hr. reaction of 26.5 g. CII,:CflCN
with 178 g. McEtCO in the presence of MONa In EtOll gave
.27-30TO -jxelylvalcronilrile, bu 110-11% nj? 1.4355, which
'a and 20.8 g,
refluxed 30 hrs. with 30.5 a. IICChN
HCChH shnilarly gave 74% 24-diurethyl-&piperidone, m.
W. Dry MePrCO(109 g.) treated with 3 ml. 10% MONa-
EtOff, follc~wed by 17.1 g. CH,:CHCN added'overi-Ults.-
and heating 6 hes. on a stealn bath, gave aftdr neutriliza-
tion with AWH 26% -i-aedy1cabrarilrde (1) , b, nl,* .
1A381,clatt.0624. To3Gg. AcCFIl-tCOjCt and 4 tal. 10'3'
a
EtOlla-BtOH was added at 10-12* in 15 rnin. 10 g. CHI:-
CHCN; after 4 hrs. the soln. was acidified with AcOH and
-distd. yielding 71% 7-a4retyl-y-carbethoxycapronitrile, bo
164-4.5*, nj,6 1.4502, d2a 1.0518, which refluxLd 4 brs. with
aq. Na2CO3 gave 21% 1. bA 142-3'. 1 (11 Z.) refluxed 40
hrs. with 18.4 g. HCOtH and 27.1 g. IICO~Na then treated
with 12.2 g, HCOJI and refluxed 23 hrs., gave after usual
treatment 60% 2-inethyl-3-ethyl-6-pij>l!ridone. b,. 152-5*,
VEC)uCTION \,%ill-W for?,m~c KID
tit. Sitnil;trly -r-mri hyl-, - i4tibul yrylvaleri suit rile
gave MV;, in. I I I- J2*.
Similarly 10 g. reflim(l 21)
.1irs. with 10.1 g. 11CO111 and 23.8 g. BCOAL gavu 72,/,,
traits-ortahydro--qtiiiiola,-ic, in. 151 '; Vionclallydro deriv. is
fortried with 1lCWl aloine. Hvilioxisig the pr(Rhict with
coned. 110 5 lirs. gave acid-
l1a, In. 173-1*, frons which %vas prel)(1. 1rams-#-(Z-bcij:-
artridacyclobcxyl )propi(potic acid, in. 2(K)', by acti;)n n1alIZO.
To 10 g. lJzC[I,Cll..Crl.', 200 ttil. 3% 01, tit 12 11. 6 Ar
' It
NaOlf was added contigh MOll to form a sobi., which
heated 5 lirs. sit ~., yielded after concti. and neutrali-
zation 45"NO BzzC11jClIjCON1I2~ tit. 125% a 30% yield te-
sulivi front keeping the isitrile in concd. 11,90;_2 firs. Ths;
asmide (5 g.) refluxed 40 Ism with 10.2 C. 11COiNa and 7 g
flC02H gave after cooling, remov, t
al of tar and add ." ?
coned. NaOH, a resirions Inass which heated. briefly vgitjjjN_
FICI gave 30% 2-phertyl-6-pyrro1fdone, tn. lG8%,,fl1W , ,
fluxed 10 lirs. with coned. 110 gave '),-amino-Y-Ae a j;9
acid-Ila, tit. 179'. 'r
Benzoylpropionitrile ursder.t. 1~fQqfriivc
condit ons gives but a very pt)or yield of the ph'_Yl~y~
rolitione owing to formation of touch tar. Heating
benzoylproplonitrile with 11CON11% and a little HC%NI14
---7-
6 hrs. at IW* gave a red solid. decomp. 250*. G. M. F1_
. ___ ____ . . . _.- _i
USS~/ Orga*nic Chemistry - Synthetic organic chemistry F~ 2
Abs Jour Referst Zhur - Khimiya, ~jo 4, 1957, 11792
Author Mikhaylov RX., Vavar V.A. (Communication 8)
A1,11khaylov B.Y., (Communication 9)
rnst Department of Chemical Schiences, Academy of Sciences USSR
Title Organic Boron Compounds. Communication 8. Synthesis and Properties
of Dinr-yl-Borfc Acids. Conn nication 9. On Action of Phosphorus Pentachlo-
ride on '~stnrs od Dialkyl-Boric and Alkyl-Boric Acids. Synthesis of
Dialkyl Borochlorldes and Psters of Alkyl-Chloroboric Acids.
Orig pub Izv. S-SSR, Otd, khim. n, 1956, No4, 451-456; 508-509.
Abstract Communicntion 8. Description of synthesis of (9~ -C 10F7)
BOH (1),
2
(p-BrC 6H4)2 BOIT (!I) and (p-ClCF4)2B(Off).H20 (ITT) and study of the
properties of the acids and tha~ir derivati,,es. ( ~~-C
-iso
BOC
H
H
)
7
lo
2
9
4
(IV), (p-BrC F BOC4Ha-isO (V) and (p-ClC H Bnc H -iso (171) were
6 4)2
6 2
4 9
Card 1/6
USSR1 Organic Chemistry - Synthetic organic chemistry
Abs Jour : ReferaL Zhyr - KhimLya, No 4, 1957, 11'(92
E-2
Residue after removal of solvents Ls diluted with isopentane, yield of
iv 63%, mp io4-1050 (from n-hexane). From filtrate, esterification of
remaining iso-C4H9 OH, were obtained 15% (c>~\ -Cl0H7)BOCkHg-iso, BP 166-
i68o/6 m., d20 0.9777. To a suspension of 10 g IV in 20 ml CH OH are
' 4 3
added 15 MI of 30% NH4 OH. Obtained 97.5~ f(cx~ -ClOH7 )2 B(OH)2 7 NH 4
(XI), MP 10-7-1080 (from CH OH). Suspension of 4.94 g XI in 30 ml e-
ther acidified with 5 ml HK (1:1). From ether layer isolated 71.7%
I, MP Ilk-5-1150 (from petroleum ether). Solution of 2 ~g I in 5 ml
'�0C1, boiied 2 hours. After removal excess SOC12 obtained-98% x, mp
190-1920 (from benzerte-t-petroleum ether). From 0.65 mole p-Brc6H4MgBr
(I M solution) and 0.25 mole VII, after stirring for 8 hours at
0
-75 , treatment with 450 ml of 5% HC1 and esterification, were obtained
39% V, BP 161-1630/1 mm, (in N2 current) and 37% p-BrC6 H4 B(OCHg-iso)
BP 109-1100/1 mm, d20 1,1583. 2.25 0a V mixed by shaking with 5 ml 30%
4
Card
USSR/ Organic Chemistry - Synthetic organic (-hemistry
Abs Jour : Referat Zhur - Khimiya, No 4, 1957, 11792
E-2
washed with water and dried over CaCl . Yield 1.1 g, MP 706-780 (repri-
cipiLated from alcohol with water ). 22.85 g VI dissolved in 8.4 ml
1.09 N NaOH. Water slowly driven off in vacuum at 60-70' - Residue
washed with C6H6' Obtained 2.2 g (kP-ClC6H4)2B(OH)2)Na (XV). From
0.3 g XV isolated on acidification 0.25 9 111.
Communicat-ion 9. Study of interaction of PU5with (n-C09)2BOC4H9-n
(XVI) and with (n-C H Vn-C H )BOC4H9-n,(XVII). Reaction with XVI-or
4 9" 3 7
XVII takes place with formation of (n-C),H,,) BC1(XVIII) or, respectively,
7 2
(n-C,,H9)(n-C3H7)BCl (XIX), C4H9Cl and POCI 3' It was also found that
(n-C H)B(OC H -n ) (XX) and (n-C H )B(OC H 1) (XXI) react readily with
one equivalent of PC1 5' forming, respectively, (U-C3H7)B(OC4H() -n)Cl-
(XXII) and (n-COOB(OCO 9-n)CI (XXIII), C4H9Cl and POCI 3' To 16.8 g
Card 5/06
MIKHAYLOV, B.M.; KDZNINS"iA, T.K.; BIA)KHIIIA, A.N.; SHCBEGOLEVA, T.A.
3oron organic compounds. Part 10. Complex nature of salts of boron-
-organic acids. Izv.AN SSSR Otd.khim.nauk ne.6:692-695 Ja 156.
(MLRA 9:9)
l.Institut organichaskoy khimii imani N.D.Zelinskege Akadamii nauk
SSSR.
(Borozium salts)
7
% 7
Xom
ou
ad. ERM
401-b
vim.
Z2
I awr
ao 27.4
k. Bul. 40-*~i,`. dlit I== 3,
the O*t. was Wt dvir~kbt.
dr*:HCJ, Mitri&'41 Uhagd" an'-d dlstd;;'thci-fraW
5b,kim,tvith 10% MOU4 laVerst vwvt"
Od;'4nd a freed. a -B&0 - SZ 1w by; -
tbe ort. yer. vm V
;dbtn
he reswiti *is*ad 'the orw~
WA
Layer -wh" - _s -4 opkaux dried *bth! id . . .
fratitAM -g4 Ll -iMth. $0, g. lhiM~ M hBpr.-
a gave- 90'~ I
'bi W904, 7
"d,3.5 ti-tivreactcA cker.- Purv!~B;jiBpr b, 7 -
20-plktoccu"i.. evqmu~obt n6d 'Ible -Amt. of
an appred i
PrtR, bt, WXr4* ziind'Rd,'& b%i'W8* `~ 9 ~-_ 11MAWEMI
ve
fiout AE
Whkhw"l iia::
ba'6744, The YqLs 0
p
32,~j
tech-
(d. Sode'r - d Win;
i0i , At
5
wque.- ne sawpl& is~ t 1
"ficuou
is ~ddecl 2 5S ifil 30
sobsbdei~ therp
%R ov
vii H'
-the mixt. reffimed 20'
ialn
m cl
_W20' - H
c1
Od ieffined 4p mmi"On- 9 e =cm $3
'th-miethy'Varittie indlcaipr_~
neutrathed by N ' XaOH'W~
i tkateO with tunidtol and tiimttd witb 0.10 NiOff with
phpd1phthatein Indicaton M. f~~q!qof
ff
611 CZ I - .~:. -
:~t 4-
9MUS) itir -b the"
.
I'Mit
Diatri
~~JI42C low. A -Mi" 1957.
j 10804; cf. C.4. 50, M-4k; 52i 4 -Ta 156 g. B(ObU~
-
, in 400 mi. 1340-was added at -76 ovef 0 firs., EuAgBr
Wit 80 t. Mg and on the follrMug diy (all opciratlows
ituder X) the mixt. treated with dfl.. HC4, andthe &j. layer,
HtjO, and slowly diAd, with BU0,11tintil the temp.
:
till
t
EfR
OB
dl
h
d 11P y1
l
ll
53
)
i
s
a
e
reac
e
c
x
%-
uir
j,
(
bf 70-10, din 0.8m. Shuilady-was
pd. 50% ife-Pt.
11(021u)i - bi: 7"50, do* 0.9107.' of-&W
(OBu)t And hexyl We. gave 83.5% R~B(OQffi;N, %~ 180-1
-
Um 68m-;'A4W1Y- prepd. OM CAOt
was
b
/0 ~PrB(O
-
.
'
F
1~1 b4
130--I~i dit O.M. iiiii! 72%1iv-PrB(DC-1+H~1 In,
added-ove;
(6 OWM' To 28.15 1411(913u)i
*
13C4 ding
31.8 YW
dbitn; 78% (OBu)CI, bo~ 40-1
&0 1; 0
9030
B
ct
d P
i
-
.
u
an
.
=. S
milar dn; t 32,2
,
hof55 .-PC114124rcemars Shr A&
Rave
WCh, b. which ignites 'm lik'ah4
49. is 61sity by~
ed- 40%,vioMfrom-17.5g.11t.
drolyzed; the sm orm in
B(OBu)CI owl',24.5
PC4~ EtB(OCjlu), (54,g.) with.,
'
P". 3 4 , EtBClj, 19.5 g.,-EtB(OCJf,z)Cl,
)
40.5 g. gave
i
-
35-
-11tB
E
OC
H
h(31
2
fOCH
-
. bit 63-5% &u4
tB
uh.
s
u
g-)
j
1%
(
PrB C72. b~ 73-V, which also 7
with 51.8 C.~ PCh gave 73.6
'
g.' iso-PrB(OCjHu)j, and
ignites Similarly, .5 ~
:
543'
hich
i
PrBC
70
7
b
so~
.
.
, w
e
46.7 g. ~PCII
hj
0%
-M.-AlikhaHoy apdR. M
hettylborazoles B
'
~
m~
.t
Md. IIM--5; - cf.
CA: Sli 49&ih.~T-A
'.St
'
:
Cilis was added at -30* 313 j. PhBCls in 30 ipl; C411s
and alter wariniag to rooin t6bp.,2 hn.-.the mixt. h1t&rcd
'
Hj.RC1 and evapd. yielding 3.5j. B,B,B-4ripkmy?-
front EtTN
..... NNN4rirjhy1botasc1e. m 200-3*; themother liquor from
. this gave -Ph#(XHM), 4). b. d. 0.9.24, -16- 1.5120;
ev
I LO,
the latter i readily attAci&d HC and atni. 0. The
'
after the-dista. gave ix~e triphenyltriethylborazole
reudue
for a thtal )icld, of, 21%; thi.pure substance. ra. 205-7
- the boraxele is stable in air a-
etr
;d is slowly
ether)
(CH
.
.
rp
;
-attacked by hot alk. HIC4. . Heating I to 210* 2 hrs. gave
17.3% triphenyltrieftiborazole. Addfi, of 12.7 g. PliBCI,
to'29JS'rfil.*PhNHz.in. CA as above gave 64.7%-.PhB.
(NYAN, - in. 83.5-15V (hexane-Isopentane); wWch - is
rapidly - hydrol aed. by R:O.- Heating th6s ~ ta ~270,* -gave
m. above
'R, sibailar ylaye- ;I
-ThuCh indwRtsN W;i-r" 14
(C
IV
:
2 'd -_--t'under
00-2 AM*ork
W
ba
ft
L
.
~
ow Zth;dg of siutheds of ber ii arlyatives"
Mlkhallov' and 'T. V. lbid.
11264 _P_
'.MeCjH4B(OCH 48.8 g. PCIs -gave
'
Rtf,)i b. 113-45%, V
U
1.5017,GOMIO.~, (iso-Bu0)BPhCI (17.3 g.) treated with
NHi in RtsO gave after sepn. of N134CLanA cliapa. 3.85 g.
B B B-iriphoxylboasote, n!. - 180-2", Rhd "70% FhB(OBU-
12+46; - Paxe - triphoylbor4sole tn. 1814.5*
gcj-h-isopintane~; -Ahm in C61F. with NHs gave 00%
I osik the appropriatc. chlow estera.,8a% BX
54r"4ajyj~
,
~bomwk, m. JW~WO; Od: 84.p% !ri(IwxapmhYj)bVr4zpk M.
:185-7.1 WbUe the, dse of a P" ropliate mines gave 72.0 ar
d 2
4
.
an
7a
in-
M
Kosolavoif
G
P,
t7 .
.
,AUTHOR3: M_ikha.viov, B, M , Shchegoleva, T AL. sov,162-58-6-2311377
TITLE: On the Effect Produced by Primary A-mines Upon the -,,'sters of
A','-1-`-1oroborJ_c Ac id P deystvii pervi_-hnykh aminov na ef iry
a?J-c4_1khkr`bornykh kislot)
PERIODICAL: Izvestiya Akademii nauk S33a, Otdeleniye khimicheskikh nauk,
1958, Nr 6, pp: 777--779 (USSR)
ABSTRACT: In the present report the results obtained by the investigation
of the effect vroduced by primary amines tof ethylamine and
aniline) and upon alk~l-chloroboricc acid are described. Under
the action of these primary amines 'he esters of alkyl-
chloroboric acids are transformed into esters of the alkylic
boric acids and into U-substituted alkyl boron diamines
(formulae I-IV). Reaction develops by way of the stage of
amino-ester formation (IV '), This ester is symmetrized either
in ester and initial diamine or it reacts with the 2. alcohol
molecule:
n- C H B(NHC,--i + POH-, H BNHC H (OR)]
4 2 4 9 1 2 5
ROH
n- c H B(NHC H n H B(OR) or n-C,H b(0?,) + C H NH-,
Card 112 +
.1 9 2 5 2 4 a 2 2 2 5
,On the Effect
Eater's of Alkyl-Cifiloroboric
ASSOCIATION:
SU2',IITT-"-'D:
Produced Frimry Amine.3 Upon
Acid
There Sov:Let reference.
Insti-tut organicheskoy khimii
sikademii nauk 3j6i (Institute
N. D, &-insk"y,Aj USSR)
January !7, 1958
tile ~'-'GV /62-58-- -23/37
im. N, D. Zeiinsko~,o
of Organic Chemistry J-meni
1. Alkil chi -obcr-`3 Lc~-'d fn-~,al -e ti
C
2. ArrI7-*---ie-----.-.he:n~-c-."-
%.lard 2112
A `_~ T H' C- RE 3. 21. , Shci'.et~oleva.- T. A, SOV/62- 58- 7-11 1/26
TITLE~ Organic Bcron Compounds Bororganicheskiye soyedinen4-ya)
Communication 25: On the Action of Organic Acids on the n.Butyl
Esters of n.Chlorc Propyl Boric Acid (Soobshcheniye 25. 0
deystvi~ or-'anicheskikh kislot na n.butilovyy efir n.propil-
1-h1orbornoy Visloty)
PEHIODICAL~ izvestiya Akademii nauk SEER, Otdeleniye khimicheskikh nauk,
11958, Nr 7r pP 6t)0 865 (USSP)
A'~2'STRACT_ The properties of the esters of chloro aryl boric acids and
-hioro alky! boric acids'produced by means of the interaction
of ecuimolecular amounts of esters or organoboric acids and
phosphorus pentachloride)(Refs 1,2) have hitherto been little
irvesti,gated. In the present paper the results of the inves-
tigation of the reactions between the n.butyl ester of chloro
pr,):~.yl boric acid and organic acids is discussed. On the action
of' acetirl-- acid cn the butyl ester of chloro propyl boric acid
t~,e n.bu~-y, esters of n,butyl boric acid, n.boron propyl pyro-
acetic ~In-'nydride ' chlorobu-~yi and butyl acetic ester are formed.
C a r d I By tl,.c- action of propionic acid on the n.butyl ester of the
B:,~f~~n Cc.--.-- --inds, Com:nunicl-tion 25: On the SOV/62-58-7-11/206
licti.on of 0---Eanic A:~~ --!~ on tne n.Butyl Esters of n.C'~'-,Dro Prozyl Boric Acid
nichlo-3 boric acid the r.but-'! ester of n.propyl boric
ac4('- n.lror: prr)pyl p- ro
r-de, chlorobutyl
and buty! ester of' propionic -icic are furmed. The au-.hors also
ex-,)Iair~ed th~- Mechanism of the r,1-aotiGrsbetvfeen organic acids
and the ester of n.chloro propyl boric acid. The n.butyl ester
of n.propyl borio acid reacts with acetic anhydride in the
presence cf :ydroE,en chloride with a simultaneous formation
of n.boron propyl pyro acet-.c anhydride, butyl acetic ester,
chloro butyl and chloro acetyl. There are 6 references, 4 of
which are Soviet.
AS SOC I AT I ON, Inst-'tut or.-anicheskoy khimii im.N.D-Zelinskogo Ak&dP-mii nauk
SSSR(Institute of Or,,-ar;ic Chemiistry imeni N.D.Zelins'--Ci3~,AS USSR)
SUBMIT-TED; De-ember 23, 1956
Card 2 !,2-
t~ n! L, A
A -
TIT T
1 t r a 1.z L; 1 d o v 1 -ii., t4 11
l'-~v':.Alja A~' S j it- ri~
12 -1 j~3 :;~ )
~ted a na-ber cf on-aziolboron cc,:,,
of :,ere for ti.Q first ti~-,e obtai-L-d in ruf,r~mnci2 3) for t'le
'f det,r;.-'iniri~; t7it:~ joszibilitj ----f -.sin-~- t`.el.l f---r ti,.e ru-
Ck'-:-'Ai'!.L: of 'fhC1 c~-~tcrs z)f an(~ d-il.~ 1 'b L, r c
till ttof a :)eca-u ov-~-nt ~le
i n t u i t t t i 11: t -i 0 f 1:-L t t t
~;~iai. ~c. Ti-
y 1 b j r:]L t,:; a S'~~ n ra C t i C c f, n -i ~3 r ~Sizs
Qlc t:le -tt~r -j.~lut J, ;0 It
4 t t C. ~; t -- r s 0 r, d I 'I- C Z- i 0 a i C C
irlltrud,ictiun inito a a
t'lc lat-'.Or
ioboron co:,-,,,:.uids wit:i ar,;-l-L3u:,stitAcnts t;-"~ a
Card 1; Weal
C
1 n v t i,
ASSO'T'I 10',': Inst.; tute
~I:-titat
In-tit-ite
in--titat
f ur Or-anic imeni N.D. Zelinskiy AS USSR
or,
for Ph.,~s i_--. imeni P.N. Lebedev AS USSR
V!, T 1L' T; b~-r-- of ~on-ress
1. Chemistry 2. Boron compounds-Application
i: d -2. -2
11IFITINA, A.11.; GALANIN, M.D.; ARONOVICH, P.M.; SHCHEGOLEVA, T.A.;
miKHAnov, B.M.
Analysis of scintillators containing boron organic compounds.
Izv. AN SSSR. Ser. fiz. 22 no.1:14-20 Ja 158. (MIRA 11:2)
l.Institut organicheakoy khimii. im. N.D. Zelinskogo AN SSSR i
Fizicheskiy institut im. P.N. Lebedeva AN SSSR.
Odintillation counters)
(Nuclear physics--Instruments)
SHCH-EOCIZITA, T. A., Candidate of Chem Sci (d-iss) -- "--hp- s7nthesis and trans-
formation of organoboron compounds of the aliphatic series". Moscow, 1959. 9 pp
(Acad Sci TTScz-R, Inst of Organic Chem im N. D. Zelinskiy), 130 copies (,KL, Tio 21,
1959, 11-P)
5(3) SOV/162-59-2-30/40
A.UTH,CM: IMikhaylov, B. W., Shchegoleva, T. A.
TITLE: --.'ffect of Selenium on Boron Trialkyls (.Deystviye selena na
bortrialkily)
PEiIIODICAL: Izvestiya Akademii nauk SSSR, Otdeleniye khimicheskikh nauk,
1959, Nr 2, pp 356-357 (USSR)
A,JSTiACT: In the present news in brief the authors report on the behavior
of boron trialkyls towards selenium. It was found that they re-
act with selenium in a very peculiar way. On heating of the
mixture of tri-n-butyl boron and selenium a gradual decomposi-
tion of selenium was observed at 220-250 0 which is accompanied
by an i.ntense separation of gaseous products. As a result of
the reaction C 8 H18B 2Se5 is formed. On the hydrolysis of this
compound n-butyl boric acid was precipitated which indicates
the occurrence of a B-C bond. It is assumed that the compound
obtained has a cyclic structure(Ref 1). According to the rules
for the nomenclature of saturated 5-membered heterocyclic
systems (Ref 5), this compound was called 3,5-di-n-butyl-3,5-
(card 1/3 diboron-1,2,4-triselenolane. The gas separated during the re-
ESfect of Selenium on Boron Trialkyls 6OV/'62-59-2-30/40
action contains hydrogen and butylene. The reaction proo-c-eds
according to the following equation:
2(C H ) B + 3Se - 4C F1 + 2-H + Se - Se
4 9 3 8 2 1 1
C4H9 -B\ / B - C 4H9
Se
A similar reaction takes place on heating of triisobutyl boron
with selenium, wherein 3,5-diisobutyl-3,5-diboron-1,2,4-tri-
selenolane (II) is formed. 3,5-dialkyl-3,5-diboron-1,2,4-di-
selenolanes are yellow viscous liquids. They are very sensitive
to atmospheric moisture and oxygen. By the influence of n-butyl
alcohol uPon 3,5-di-n-butyl-3,R,-diboron-1,2,4-triselenolane
metallic selenium, hydrogen selenide snd n-butyl esters of the
n-butyl boric acid are formed.
Se - Se
I I + 4C4 It 90H - 2C4H9B(OC4H9)2 + 2H2Se + Se
C4H9- B\ 4ti9
'3e
There are 3 references, 1 of which is Joviet.
Card 2/3
Effect of 3elenium ozi Boron Trialkyls sov/62-59-2-30/40
ASSOCIATION: Institut organicheskoy khimii im. N. D. Zelinakogo Akademii
nauk SSSR (Institute of Organic Chemistry imeni N. D. Zelinskiy
of the Academy of Sciences, USSR)
SUBMITTED: July 91 1958
Card 3/3
5(3)
A~'THORS: Mikhaylov. B, M., Shchegoleva, T. A. SOV/62-59-3-25/37
TITLE: Synthesis of Trialkyl Borons With Functional Substituents
(Sintez bortrialkilov s funktsionallnymi zamestitelyami)
PERIODICAL: Izvestiya Akademii nauk SSSR, Otdeleniye khimicheskikh nauk,
19'~9, Tir 3, pp 546-547 (USSR)
ABSTRACT: This is a brief communication on the investigation of the
reaction of diborane with vinyl-ethyl ether. Tri-(2-ethoxy-
ethyl)-boron (I) was obtained in insufficient purity as a result
of this reaction, Probl-,,bly, in this case the reaction is compli-
cated by side reactions, In reference 6 it was shown that the
lowest alkyl group may be easily replaced by the highest one
if the mixture of the correspondincT trialkyl boron and olefin
is heat6d and the easily volatile olefin is removed from the
reaction mixture. The authors extended this reaction to un-
saturated compounds with functional substituents. By heating
triisobutyl boron with 2-chloro-1,1,2-trifluomethyl allyl
ether (II) tri-r3-(21-chloro-11,11,2'-trifluoroethoxy)propylI
boron (III) was obtained in a yield of 52 ~', Triisobutyl
boron reacts also with unsaturated organosilicon compounds.
Card 1/2 By heating triisobutyl boron with allyl trimethyl silane or
Synthesis of Trialkyl Borons With runctiona-1 SOV/62-59-3-25/37
,Substituents
allyl trichlorosilane tri-0-trimethyl silyl propyl) boron (IV)
and tri-(3-chlorosilyl propyl)boron (V) were obtained according-
ly in yields of 62-69 %, The investigations of the synthesis
of functional trialkyl boron derivatives according to the
mentioned method are continued. There are 7 references, 1 of
which is Soviet,
ASSOCIATION: Institut organicheskoy khimii im, Y, D. Zelinskogo Akademii nak
SSSR (Institute of Organic Chemistry imeni N, D. Zelinskiy of
the Academy of Sciences, USSR)
SUBMITTED: July 9, 1958
Card 2/2
5 ( 31 )
A T: T 11 MR Shc'-.egqj
A. SOV/62-59-8-8/42
o'likhaylov, B.. M, ,
~
va,.
e
T
_
_
,
_
_._
_
TTTLE-, Boron-organic Compounds, Communication 42: Alkylpyro-boro-
acetic Anhydrides
~-IERIODIC.A:L: Izvestiya Akademii nauk SSS11. Otdeleniye k1limicheskikh nauk,
1959, Tir 8, pp 1395-1396 (Tj-ssR)
APMPRACT: It was shown in the present paper that the mixed anhydrides
of flatty acids and n-propylpyro boric acid normally formed
under the influence of organic acids unon esters of n-propyl-
chloro boric acid may be obtained much -more easily by heating
alkyl boric acid with the anhydride of a3etic acid over a
water bath. In this way it was possible to synthesize the
anhydrides of n-propylpyro-boroacetic acid M, i-sopropyl-
pyro-boroacetic acid (II), and n-butyloyro-boroacetic acid
(M) as well as isobutylpyro-boroacetic acid (IV), with
yields ranging between 60 and 70a of the theoretical yields.
The compounds obtained were investigated as to their different
reactivities. It was shown that the anhydrides of alkylpyro-
boroacetic acid easily react with the esters of alkyl boric
acid at 160-1850, forming the anhydrides of alkyl boric acid,
Card 1/2 The anhydride of n-propylpyro boric acid forms a mixture of
Boron-or.-anic Compounds. Communication 1,1t2: Alkylpyro- SOV/b2-59-6-8/42
boroacetic Anhydrides
anhydrides
the esters
pyro boric
the esters
part the reaction
reference.
of propyl and phenyl boric acids when heated with
of phenyl boric acid. The anhydride of n-propyl-
acid forms anhydride of propyl boric acid also with
of n-propylchloro boric acid. In the experimental
method is described. There is 1 Soviet
ASSOCIATION: Institut organicheskoy khimii im. N. D. Zelinskogo Akademii
nauk SSSR (Institute of Organic Chemistry imeni N. D. Ze-
linskiy of the Academy of Sciences, USSR)
SUE'lITTED: November 21, 1957
Chrd 2/2
5-0) SOV/79-29-9-.681/76
AUTHORS: Mikhaylov, B. M, Shchegoleva, T. A. I
TITLE: Organoboron Compounds. XLVI. Malkyl Boric Acids and Their
Derivatives
PERIOnICAL: Zhurnal obshchey khimii, 1959,, Vol 2Q,., Nr 9, pp 3130-3135
(USSR)
ABSTRACT: Alkylborates may serve for the synthesis of symmetrical and
unsymmetrical dialkyl borates. The butyl esters of di-n.-butyl-
and n,propyl-nbutyl boric acid were synthesized by reaction
of nbutyl lithium or m-propyl lithium with the rb,,butyl ester
of n,butyl boric acid (Ref -11). Based on this method rL-butyl-
ethyl-n-butyl borate and n,butyl-ethyl-n..-propyl borate were
obtained here according to the scheme:
Li !> C
+ C
H
+ C
H
RB(OC
H
EBOC
H
H
OM,
)
2
2
9
2
4
5
9
9
5
4
4
where R = C
. n.--C
H
H
' The synthesis of dialkyl borates
9
3
7
4
on the basis of alkyl borates can also be practiced with
organc-magnesium compounds. Thus; a 45% yield of nbutyl-di-
n.-propyl borate was obtained by reaction of n.-propyl mag-
Card 1
V-3 nesium bromide with n.-butyl.-n.-propyl borate-
SOV/79-29-9-68/76
Organoboron Compounds. XLVI. Dialkyl Boric Acids and Their Derivatives
n.-C3H7B(OC4H9)2 + n.-C3H7MgBr ~O (n.-C3Er 7)2 BOC4H9' The
dialkyl boric acids resulted from saponification of dialkyl
borates. The stability of dialkyl borates to hydrolyzing
agents is conditioned by the nature of the arrangement
0f esters(for examples see references 8, 10). In this regard,
n.-butyl dialkyl borates are much more stable than glycol
esters (Refs 12, 13). The reaction of n.-butyl-di-n.-butyl
borate with a 10.1 caustic soda solution with subsequent
acidification is shown by scheme 1. Butyl alcohol is also
completely eliminated together with water in the concentration
of a salt solution (I) gently heated and distilled in vacuum.
The crystalline residue is a sodium salt of di-n.-.butylborenium
acid (II) in analytically pure state. The reaction process
of the formation of salt (II) is explained by scheme (2).
Di-n-butyl boric acid (Scheme 5) results from acidification
of salt (II) after an intermediate stage of acid (V). Di-n.-
propyl boric acid and n.-propyl-n.-butyl boric acid are
colorless liquids tending to pass over into the corresponding
Card 2/3 anhydrides Then they are heated. There are 14 references,
SOV/79-20~-9-68/176
Organoboron Compounds. XLVI. Dialkyl Boric Acids and '2heir Derivatives
4 of which are Soviet.
ASSOCIATION: Institut organicheskoy khimii Akademi-4 nauk SSSR
(Institute of Organic Chemistry of the Academy of Sciences,
0
USSR)
SUBMITTED: July 10~ 1958
Card 3/3
MPCO/000/07/07/007
~S7 1? 3/0862
B015/BD54
AUTHORS: Mikhaylov, B. M., Shchegoleva, T. A., Blokh-ina, A. N.
---------- I
TITLE. Reaction of Tetra-n-butyl Mercapto Diborane '"ith
'Unsaturated Compounds I
PERIODICAL: Izvestiya Akademii nauk SSSR. Otdeleniye khimicheskikh nauk,
1960, No~ 7, PP. 1307-1309
TEXT: The olefin hydrocarbons (hexene-1, 0octene-1, styrene) react with
tetra-n-butyl mercapto diborane at 70-80 C in the preseme of pyridine
under formation of the n-butyl esters of alkyl thioboric acids. The
reaction between tetra-n-butyl mercapto diborane and propylene or iso-
butylene proceeds in a complicated way. On heating tetra-n-butyl mercapto
diborane with propylene in the presence of pyridine in an autoclave
at 70-BOOC and 5-15 atm, the n-butyl ester of n-propyl thioboric acid
as well as the n-butyl ester of di.-n-propyl thiobaric acid and tri-n-
butyl thioborate are formed. Tetra-n-butyl mercapto diborane reacts
with isobutylene in a similar way; a mixture consisting of the esters of
isobutyl thioboric- and diisobutyl thioboric acid as well as tri-n-butyl
Card 1/2 Ile
A2103
Reaction of Tetra-n-butyl Mercapto Diborane With S/0~2/60/000/0711071/007
Unsaturated Compounds B015/BO54
thioborate are formed. The formation of the esters of dialkyl thioboric
acids and of thioborate is explained by the fact that tetra-n-butyl
mercapto diborane symmetrizes to thioborate and di-n-butyl mercapto di-
borane, and the latter reacts with the olefins under formation of the
corresponding esters of dialkyl thioboric acids. There are 3 Soviet
references.
ASSOCIATION: Institut organicheskoy khimii im. N. D. Zelinskogo, Akademii
nauk SSSR
(institute of Organic Chemistry imeni NG Do Zelinskiy of
the Academy of Sciences, USSR
SUBMITTED: December 24, 1959
Card 2/2
69509
-7 OP
AUTHORS: Mikhaylov, B, M., Shchegoleva, T. A. S/020/60/131/04/035/073
BO11/BO17
TITLE: Synthesis and Some Transformations of Alkylmercaptodiboranes
PERIODICAL- Doklady Akademii nauk SSSR, 1960, Vol 131, Nr 4, pp 843-846 (USSR)
TEXT: The authors studied the reaction of diborane with n-propylmercaptan and
n-butylmercaptan in ether solution at room temperature and with different ratio
of the reagents. Tetraalkylmercaptodiborane is formed as a main reaction product
if a mercaptan excess is present (see Scheme). These compounds show considerable
resistivity: they do not change on longer storage, and may be distilled under
vacuum. On distilling theyturn into highly viscous liquids, but some hours later
they become mobile again. The molecular weight of the dimeric form of dialkyl-
mercaptoborane is by about 1.5 times higher than the cryoscopically determined
molecular weight of tetraalkylmereaptodiboranes. Apparently, a partial dissocia-
t:nn of the produced alky1mercapto derivatives of diborane takes place in the
benzene solution. In the reaction between diborane and n-butylmercaptan (ratio 1:2),
much less tetra-n-butylmercaptodiborane is formed. Di-n-butylmercaptodiborane
C4H9SBH 2BH2SC4 H9is formed as a main product. It is an unstable compound which
is symmetrized on storing at room temperature into diborane and tetra-n-butyl-
mercaptodiborane. The latter was identified on the basis of its capability of
reacting with olefines at room temperature and of forming n-butyl eater of dialkyl-
Card 1/3
69509
Synthesis and Some Transformations of Alkylmercapto- S/020/60/131/04/035/073
diboranes BO11/BO17 I
thibboric acids (see Scheme). Furthermore, the yield in tri-n-propylboron,n-butyl
ester of di-n-propylthioboric acid, and tetra-n-butylmer-ca-p-t-odiborane on passing
propylene through the reaction mass of diborane with n-butylmercaptan is mentioned.
The yield differed according to whether the mass was fresh, or stored for one
night. The yield in di-n-butylmercaptodiborane is very low on the action of di-
borane on tetra-n-butylmereaptodiborane since equilibrium is established between
the reagents and the final product (see Scheme). Polymers are known which were
produced from diborane and methylmercaptan in the gas phase (Ref 2). The hydrogen
atoms of tetraalkylmercaptodiboranes show much lower reactivity than 0diborane.
Thus, the reaction of the former with mercaptan starts only at 50-60 , and proceeds
energetically at the boiling temperature of mercaptan. In this connection, tri-
alkylthioborate (see Scheme) is formed. On treating tetra-n-butylmercaptodiborane
with water or alcohol at room temperature, no hydrogen is separated. Under the same
conditions, N-trialkylborazols were obtained under the action of primary amines
(ethylamine, n-butylamine) on tetra-n-butylmereaptodiborane. Apparently, a complex
of dialky1mercaptoborane with amine (I) is formed during the first stage of the
process. This complex is transformed into alkylmercaptoalkylaminoborane (II) with
mercaptan being separated. An N-alkyl derivative of borazol is formed from (II) un-
der precipitation of mercaptan. The high stability of the B-H bond becomes manifest
in the reactions between tetraalky1mercaptodiboranes and olefines. The authors
Card 2/3
69509
Synthesis and Some Transformations of Alkylmercapto- 3/020/60/131/04/035/073
diboranes B0111/B017
succeeded in adding tetra-n-butylmercaptodiborane to olefine hydrocarbons by heat-
ing the reagents to 700 in the presence of pyridine. There are 6 references,
2 of which are Soviet.
ASSOCIATION: Institut organicheskoy khimii im. N. D. Zelinskogo Akademii nauk
SSSR
(Institute of Organic Chemistry imeni N. D. Zelinskiy of the
Academy of Scienceal USSR)
PRESEIVED: December 22, 1959, by B. A. Kazanskiy, Academician
SUBMITTED: December 21, 1959
Card 3/3
MIKHAYLOV, B.M.; SHCHEGOLEVA,
T.A.; SHASHKOVA, Ye.M.
S7nthesis of alkylthioboric acid esters from trialkylborines and
thioborates. I4y.fill SSSR.Otd.khim.nauk no.5:916-917 My 161.
OffRA 14:5)
1. Institut organicheskoy khimil im. N.D.Zelinskogo AN SSSR.
(Boric acid) (Boron compounds)
SHCHLGOLEVA, T.A.; SHASHKOVA, Ye.M.; MIKHAYLOV, B.M.
Reactions of triethylthioborate with amines. Izv.AN SSSR,Otd.kh-4m.
nauk no.5:918-919 My 161. (MIRA 14:5)
1. Institut organicheskoy khimii im. H.D.Zelin kogo AN SSSR.
(Boric acid) (Amines)
I
MIKHAYLOV B.M.; SHCHEGOLEVA, T.A.
Y
Synthesis of 1-n-butylmereaptoboracycloalkanes. Izv.AN SSSR,Otd.
khim.nauk no.6tlW-11-U,, Je 161. OMA 14: 6)
1. Institut organicheskoy khiaii im. N.D.Ze-linakogo AN SSSR.
(Cycloalkanes)
25047
S106211611000100610091010
B1 181 !5220
AUTHORS: Mikhaylov, B. M., Shchegoleva, T. A., Shashkova, Ye. M.,
Sheludyakov, V.
TITLE: Polymers Pnd trimers of alk,-,,l mercanto-boranes
PERIODICAL: Akademiya nauk S33R. Izvestiya. Otdeleniye khimicheskikh
naLik-, no. "", 1 ")61 , 1163
TEXT: The aut',~n.,s stated that the reaction of diborane with mercaptans
(1:2) in ether results in r)ol.,,,mer alkyl merea-pto-bornnes. The diborane
reacts witr methYl mercavtan, forming a solid .-olymer (CH 3SBH 2)x which
had been synt-esized previously by A.Bura and R. Wagner (see below) with-
out the use of a solvent. On reaction of ethyl mercaptan or n-butyl
mercantan with diborane, glass-like polymers of ethyl Miercapto-borane
(C2H 5SBH2)x or of n-butyl merca-ta-borane (n-C 4H9S'2_1_1 2)x are obtained after
elimination of the ether by listillation. The polymers of ethyl
mercapto-bor.~ne and n-butyl mercapto-borane are ccnverted gradually at
Toom temperature to the corresponding trimers of alkyl mercaDto-borane.
Card 1/3
S/062/61 /1000100610091010
0
Polymers atil trimerS ol" alkyl ... E 1 1 P '13 212 0
The trimer of ethyl mercapto-borane (C,H SBH,,) has the following
5 - 3 -) -%72 20 =
cons tant~~ 1) o i I i n)r~ a t 94 q 6Cmrn H-) ; d i20 nD 1.5323; data
ob t'i i ""ed 41.-')0; 1~1.~7 mc)l-~cular weight (determined
act
cryoscopicelly): 217.9; 22D.2. The trimer of -,-I,ut,,l mercapto-borFine
2C 20
lecomposes on vacuum distillat;on: d 0. 1157(, ; n n= 1.5130; data
id
obtained,: Hact 2.17; 2.15; B 10.25; 10~32 /"); molecu3ar weight: 293.3;
294.9 corresponding to (C 4H 9SBH 2)3* The solid --polymer of methyl
mercanto-borane is stable; however, when it is dissolved in tetrahydro-
furan, it is c-)nverted to the trimer of methyl mercanto-borane: boiling
20 20
at 60-810C (1.5rnL,,Hg);d 4 = 1.0121; n D = 1.5483; data obtained:
17
Hact 3.46; 3.37; B 17-00; 1.30 ~o; molecular vieight: 182.5; 183.6
corresoonding to (CH 3SBH 2)3' The trimers of alkyl mercapto-boranes are
fairly stable a,-a--nst the action of air anJ water. There is I non-Soviet-
Card 2/3
250417
s'o62/61/000/006/009,/010
Polymers and trimers of alkyl... B118/B220
bloc reference. The reference to the English-language publication reads
as follows: A. Burg, R. Wa.-ner, J. Amer. Chem. Soc. 705, 3307 (1954).
ASSOCIATTOT~1: Institut or-anicheskoy kh-imii im. 'T. D. Zelinskogo SSSR
'Institute of Organic Chemistry imeni N. D. Zelinskiy USSR)
SUB111ITTED: Aoril 20, 1961
Card 3/3
8,9733
S//020/61/136/003/019/027
B016/BO52
AUTHORS: Shchegoleva, T. A. and Belyavskaya, Ye. M.
TITLE: Organoboron Compounds. Synthesis and Some Properties of
Tri-(ethyl-mercapto)-diborane
PERIODICAL: Doklady Akademii nauk SSSR, 1961, Vol. 136, No. 3,
pp. 65a-641
TEXT: The authors report on the reaction of diborane and ethyl mercaptan
in eThereal solutions at room temperature.They obtained a 60-70% yield of N
tri-(ethyl-mercapto)-diborane C2H 5SBR 2ER (SC2H5)2 (1) independently of the
quantitative prcDcrtion of reagents. (I) is a liquid which can be distilled
in vacuum without decomposition, and does not dissociate in solutions.
The substitution of the remaining three hydrogen atoms by ethyl mercapto
groups is only of advantage between 110 and 1500c; in this case triethyl-
0
thioborate B(Sc 2H5)3 (11) is formed In good yields. Ethyl amine complexes
of di-(ethyl-mereapto)-borane (C 2 H5S) 2BH*NH 2C2H5(111) and ethyl-mereapto-
Card 1114
89733
Organoboron Compounds. Synthes-'s and Some S/02011'61/136/005/019/027
Properties of Tri-(ethyl-mereapto).-diborane B016/3052
bcrane C2TIT5SBH 2' NH2C2H5(IV) are formed first by the action of ethylamine
on (I). Then etfiyl-amino-ethyl-mercapto-borane (V) forms from (III) by
seDaration of mercaptan, and is then condensed into N-triethyl borazole
(VI) (see insert scheme). Ethyl meroaptan is also separated by (IV) which
is converted into ethyl-amino-borane (VII). The latter is isolated from
~Ihe reaction mixture especially in the form of a trimer (VIII). As regards
its chemical properties, (VIII) is like the trimer of methyl-amino-borane
(.Ref. 2). However, there also exists a dimer (IX) of (VII) which together
with (VIII) is contained in a liquid fraction with a boiling point of
85-900/2 mm Hg. When left standing, (IX) Is converted into (VIII). (IX)
differs from (VIII) as to its chemical properties: when heated, both are
converted into N-triethyl-borazole (VI), in (IX), however, only at lower
temperatures (partly already when distilled in vacuum), while in (VIII)
no hydrogen is generated below 140 - 1500C; at 1800C it iS COMD!etely
transformed. The behavior of (I) in Dropylene is like that of
di(n-butyl-mercapto)-diborane in ethereal solutions (ief. 1): the one half
of its molecule which is more intensively hydrogenated accumulates on
Card 2/4
Organoboron COMDounds. Synthesis and Some S/020/61/136/003/019/027
Properties of Tri-(ethyl-mercapto)-diborane Bbl6/BO52
propylene already at room temperature. Thus di-n-propyl-thioboric acid
H ) BSC H forms. The other half of the molecule is
ethyl ester (C
3 7 2 2 5
dimerized into tetra-(ethyl-mercapto)-diborane (C H (XI).
S)2BHBE(SC2H5)2
2
5
At room temperature (I) does not react with ethylene or octene. By boiling
(1) in ethereal solutions with octane, the authors obtained an ester
mixture of di-n-octyl-thioboric acid (C H ) BSC H (XII) and
8 17 2 2 5
n-octyl-thioboric acid C 8H17 B(SC2H5)2 (XIII). This accumulation is
accompanied by a symmetrization leading to the formation of (II) and
tri-n-octylboron. There are 5 references: 2 Soviet and 2 US.
ASSOCIATION: Institut organicheskoy khimii im. N. D. Zelinskogo Akademii
nauk SSSR (Institute of Organic Chemistry imeni N. D.
Zelinskiy of the Academy of Sciences USSR)
PRESENTED: July 7, 1960, by B. A. Kazanskiy, Academician
SUBMITTED: July 4, 1960
Card - --------- ----
.3/4
3/062 '62/000/003/006/0 14
3117,73144
B. S~,~Lheg~v a T. A., and Bubnov, Yu. N.
Organoboron compounds. Communication 92. Refractions of
the bonds of boron with some elements
-ODICAL: nauk
SSSR- Izvestiya. Otdeleniye khimicheskik"i
nauk, no. 1962, 413-4r19
TEXT: Refractions of (3 C), (B - 0), (B - N), (B - S), and (B - Cl)
bonds were calculated from molecular refractions of various organoboron
compounds havine re.~-ard to hybridization according to Denbigh's method.
Ahere lossiole, compounds of the type BX were used. Molecular refral-tions
&1 3
-were determined from the -~~orentz-Lorenz law. For the bonds B - C aliph. and
B - C), the mean value of their refractions was found from molecular
refractions of boron trialkyls and trialkyl borates: R D = 1.93 cm 3 and
3 3
C a mean value of R = 2-76cm
R- = 1.61 cm respect vc For B
J arom. D
was determined from the molecular refractions of aryl boric acids.
Card '1113
S/062/o2 -'COL 0
I D/O 0 3 /C 0 '//C 14
Or,~7anoboron compounds ... 3 1 17 /:~ I -
L-4
ii.olecular refractions of triamides and N-substituted alkyl-(diamino) borons
C of' 1.97 cm f
-roduced a mean value 3 for the refractions of 3 - N. The mear.
refraction value for the B - N bond in dialkyl-(amino) borons, their
N-zub,stituted and dialkyl boryl hydrazines was 2.01 cm Thus, the mean
7
I U
rufr,tctiori value of the B - N bonds may be assumed to be 1.08 cm,. For the
B bond in thioborates as well as in alkyl- and dialkyl thioboric esters,
amean refraction value of 5.59 cm3 was determined, which is some-,.-that hie-her
than the value of ~.20 cm' determined for this bond in dIalkyl thioboric
' ds.
P
- c ~ Various orEanoboron chlorides %yere used for calculating the
refractions of the B - Cl bond. As the oroduction of these chlorides in
pure form is difficult owin,~ to their tendency towards disproportionation
and their easy hydrolyzability, the values found showed high fluctuations
and ;)roduced a mean value of R D = 6.88 cm3. There are 13 tables and
27 references: 15 Soviet and 12 non-Soviet. The -four :::ost recent
references to English-language publications read as follows:
P. Chistopher, T. J. Tully, J. Amer. 0~,em. Soc., 80, 05516 (1958);
G. F. Hennion, P. A. McCusker, j. V. Marra, J. Amer. Che-,.,,, Soc,, 809 3481
(1q,58) and T. Amer. Chem. Soc. 81, 1768 (1959); D. Aubrey, M. Lappert,
Card 2/3
Organoboron compounds.
J. C-em. Soc. 1959, 2c27.
ASSOCIATION, TnStitUt orban-cheskoy
nauk SSSR (institute of
X. D. Zelinskiy of the
SUB""-L TT ED: October 16, 1961
S/062/62/000/003/006/014
B117/31,44
khimii im. 'N'. D. Zelinskogo kkadem-1 i
O-,L-anic Chemistry imeni
Academy of Sciences USSIR)
Card 3/3
MIKHAYLOV, D.M.; MCIIEGOLEVA, T.A.; BUBNOV. Yii.N.
Organoboron compounds. Report No.92: Refractions of boron
bonds with some elements. Izv.AN SSSR.utd.kbim.naWk nc-.3:
413-419 MT '62. (~LIRA 15:3)
1. Institut organicheskoy khimii im. N.D.Zelinskogo AN SS.M.
(Boron organic compounds) (Refractometry)
39573
;5/062/62/000/007/004/013
B117/B180
AUTHORS: Mikhaylov, B. M., Shchegoleva, T. A., Shashkova, Ye. M., and
Sheludyakov, V. D.'-
TITLE. Organoboron compounds. Report 102. Monoalkyl mercapto
derivatives of borane
PERIODICALt Akademiya nauk SSSR. Izvestiya. Otdeleniye khimiche8kikh
nauk, no. 7, 1962, 1218 - 1223
TEXT: The reactions of diborane and mercaptanes in ether solution were
studied at room temperature. Independent of the component ratio, diborane
ana methyl mercaptane yielded a solid, storable polymer which dissolves in
ether and benzene, and converts into a trimer in a solution of tetrahydro-
furan. A viscous, colorless polymer was produced from diborane and ethyl
mercaptane, independent of the component ratio. The reaction of diborane
with n-propyl and n-butyl mercaptanes only yielded polymers at a ratio of
1 : 2. Trimers of ethyl, n-pro 1 and n-butyl mercapto boranes formed
spontaneously from the corre8poYdi;g polymers. The' resulting trimers are
a new type of organoboron compound. They are very stable, have a cyclic
Card'1/2
S/062/62/000/007/004/013
Organoboron compounds ... B117/B180
structure, are virtually unaffected by air, not completely oxidized by
hydrogen peroxide and are very slowly hydrolyzed by heating. They yield
the corresponding borates by alcoholysis. This reaction is slow at room
temperature, accelerating as the temperature rises. Alkyl mercaptoborane
trimers and mercaptanes only react at 100 - 1200C, 'yielding large amounts
of alkyl thioborates. 55% methyl thioborate and 89% ethyl*thioborate *ere
obtained by boiling a mixture of high-boiling-mOraaptane and trimer.
ASSOCIATIONs Institut organicheskoy khimii im. N. D. Zelinskogo Akademii
nauk SSSR (Institute of Organic Chemistry imeni
N. D. Zelinski.y of the Academy of Sciences USSR)
SUBMITTED: January 30, 1962
VY\
Card 2/2
MBAYLOV, B.M.; SHELYDAYAKOV., V.D.;_~HCHEGQUVA, T.A
.- --- L_
Organoboron compounds. Report No.106z Reactions of alkyl mercapto-
borane trimers with secondary and tiertiary amines. Izv.AN SSSR.Otd.kh:Lm.
nauk no.9:1559-1564 S 162. (MIRA, 15:10)
1. Institut organicheskoy khimii im. N.D.Zelinskogo AN SSSR.
(Boron organic compounds) (Amines)
MIKHAYLOVY B.M.; SHELUDAYAKOV, V.D.; SHCHEGOU'VA, T.A.
New types of boron salts. Izv.Pli SSSR.Otd.khim.nauk no.9:1698-1699
S 16-9. (MIRA 15.'.10)
1. Institut organichdskoy khimii im. N.D.Zelinskogo AN SSSR.
(Boron-Compounds)
S106
JY63/000/003/006/016
B10 166
PERIODICAL:
Shashkoval Ye. M.t and Mikhaylov, B. M.
Organoboron compounds. Communication 113. Reduction of
alkyl thioborates to dialkyl mercapto-boraneo
Akademiya nauk SSSR. Izvestiya. Otdaleniye khimicheskikh
nauk, no. 3, 1963, 494 - 497
TEXT: It was found that ethyl thioboratef n-propyl thioborate, n-butyl
thioborate, isopropyl thioborate, and tert-butyl thioborate react with
LiAlH in nitrogen atmosphere at room temperature to give the correspond14
4 1
dialkyl mercapto-boranes' 4(RS) B + LiAlH -4 4(RS)2B9 + LiSR + Al(SR) !1~
3 4 3*1
The yield is 7~ - 85 Reaction of methyl tWoborate withLiAlE howeveri
41
did not give dimethyl mercapto-borane but a stable complex. This was conJ11
firmed by the following reactiont (CH S) B + LiH -4 ((CH S) BH]Li. Thell-,
3 3 3 3
-boronhydride is a colorless solid
resultant lithium-trimethyl-mereapto
substance which is heat-resistanti; up to 3000C and decomposes to LiClq
Card 1/2
31062163100010037o-6~16ie
..Organoboron compounds. B101/B186
methyl mercaptane and dimethyl mercapto-borane when equimolar quantities
of aCl are added, Dimethyl mercapto-borane cannot be prepared in pure
.~condition, as it is partially dimerized even by distillation in vacuo.
RS, SR, /SR
This dimerizationt B' B, 2470, 2416 cm'-1 is 42 for
H SR H
R CR 3' 17 %'for R i-C 3H79 and 0 % for R tert-C 41i9
ASSOCIATION: Institut orfIanicheakoy khimil im. N. D. Zelinskogo, Akedemii
nauk SSSR natitute of Organic Chemistry-imeni K. D.
Zelinskiy of the Academy- of Sciences USSR)
SU1L1,:-,r.1M--,11-.- June 6, 1962.
All
d
Card 2/2
-------- -------
S/olf"163/000/003/007/018
u
AUTHORSs Mikhaylov, B. M., Dorokhov, V. A., and Shchegoleva, T. Ao
TITLE: Organoboron compounds. Communication 114. Reaction of
dialkyl.-mereapto-boranes with secondary amines
PERIODICAL: Akademiya nauk SSSR. Izvestiya. Otdeleniye khimicheakilth
nauk, no- 3, 1963, 498 - 499
TEXT: The reaction of di-n-butyl mercapto-borane with diethyl amine in a
molar ratio of 1:1 in nitrogen atmosphere at room temperature gave n-bu
mercapto-(diethyl-amino)-borane in 53 ~ yield. Under equal conditions
n-butyl mereapto-(piperidino)-borane was obtained in 71 % yield by reac-
tion of di-n-butyl mercapto-borane with piperidine. Di-n~butyl mercapto-
borane and diisoamyl amine gave n-propyl mereapto-(diisoanyl-amino)-borane,
in 85 % yield. On reaction of two moles of secondary amine with one mole
of dialkyl mercapto-borane, bia-(dialkyl-amino)-borane as formed. Di-n-
propyl-mercapto-borane and diiao-amyl amine-thus gave bis-(diisoamyl-
amino)-borane in 80 ~o yie14 and di-n-propyl mercapto-borane and diallyl
amine gave bis-(diallyl-amino)-borane in 90 % yield.
Card 1/2
3/062/63/000/003/00T/018
Organoboron compounds BlOl/B186
A
SSOCIATION:
SUBMITTEDs
Institut orfanicheskoy khimii im. X. D. Zell.nskogo,Akademiii
nauk SSSR Institute of Organic Chemistr I e i N. D.
Zelinskiy of the Academy'.~of Sciences USSR
June 6, 1962
Card 2/2
ACCESSION NR: AP3000122
S/0062/63/000/003/0816/0822
AUTHOR: Mikhaylovo B. M.; Shchegoleva, T. A.; Sheludyakov, V. D.
.TITLE: Organic boron compounds. Report, 327. Reactions of the amino complexes of
alky1mercaptoboranes with halogen derivatives of hydrocarbons and HCl
SOURCE: AN SSSR. Izvestiya. Otdoleniye khimicheakikh naukv no. 5. 1963p 816-822
ITOPIC TAGS: reac-~ion mechanisms,, amine complexes of al1g2mercaptoboranes.. HG10
':halogenated hydrocarbons
ABSTRACT: Di-(dimethylamine)borane shlts were formed by the action of halogenated
hydrocarbons and HG1 on dimethylaminealkylmereaptoboranea. 'Wheii complexes of
a3,kylimercaptoboranes with tertiai~y amines reacted with alkyl halides, the alky1mer-
capto group was exchanged for a halide groupp converting them into borane halide
Complexes. HC1 cleaved the trialkylamine complexes of alky3inercaptobo-ranes, giving
aii~ylmercaptoborane trimers and amine hydrochlorides. Dimethylamine-methy1nercap-
toborane reacted with dimethylamine hydrochloride to yield the chloride of di-(di-
methylamine)borane. Orig. art. has: 3.1 equations.
ASSOCIATION: Institut organicheakoy khimii im. N. D. Zelinskogos Akademii nauk
SSSR (Institute of Organic Chemistry, Academy of Sciences SSSR)
L 1709~663 EPR'AwP WAPF (c)/FwP (q)/EVtT (m)/BDS AFF?C/ASD Pr-4/Pc-4/
PS-41 RKt,,JW/JD/MAY S/062/63/000/004/008/022
AUTHOR: Mikhaylov, B. M., Shchegoleva, T. A., Sheludyakov, V. D., and
Blokhina, A.
TITILE: Organo-boron'A pounds. Report 116. Reactions of alkyLmercapto-
com
boranel-p=oymers with unsaturated compounds
PERIODICAL: Akademiy nauk JSR. Izvestiya. Otdeleniye khimicheskilch nauk,
no. 4, 1963, 646-651
TEXT: Inasmuch as various derivatives of diborane exhibit the capability
to be added to unsaturated compounds the authors sought to study the behavior
of allqrlmereaptoborane polymers in relation to olefins and diene hydrocarbons.
The addition of the n-butylmercaptoborane polymor to diallyl was performed,
which results in the formation of 1-n-butylmercaptoboroncycloheptane:
CH2=CH-CH2 .0, CH2CH2CH2
(n-C4EIgSBH2)x +x -*x n-C H SB %%
CHfCff-CH2 CH2CH2CH2
Card 1/2
L 17098-63
3/062/63/000/004/C08/022..
Organo-boron compounds ......
A polymer of methylmercaptoborane joins with olefins to form methy others of
dialkylthioboric acid. In the action of isoprono on a polymer of methylmorca-
ptoborane the product is 3-methyl-l-methylmercaptoborocylelopentane. A nitro-
gen atomosphere was used in all ODerations involving organo-boron compounds.
ASSOCIATION: Institut organicheskoy khimii im. N.D. Zelinskogo Akademii nauk
SSSR (Tnstitute of Organic Chemistr-v imeni N. D. Zelens1qXL_Lca-
demy of Sciences USSR)
SUBMITTED: June 7. 1962
Card 2/2
SHCHEGOU,VA, T.A.; SHELUDIAKOV, V.D.; MIKHAYLOV, B.M.
Nature of the coordination compounds formed by boron and
diborane halides in ether oolutions. Dokl. AN SSSR 152 no.4:
888-891 0 163. (MIRA 16,11)
1. Institut organicheskoy khimii im. N.D. Zelinskogo AN SSSR.
Predstavleno akademikom B.A. Kazanskim.
L 19490-65 EPF(c)/EPR/,7WA(h)/EWP(J)/EWT(m)/T Pc_4/Pr_4/Ps_VPeb RPL
ACCESSION NR: AP5002072 S/0062/64/000/002/0365/0367
AUTHOR: Shch eva, T. A.; Shashkova, Ye. M.;
Kiselev, V. G.; I ~i~ay 1 o vB. M.
TITLE: Hydroboridation of dienes with chloroborane
SOURCE: AN SSSR. Izvestiya. Seriya khimicheskaya, no. 2, 1964, 365-367
Y
TOPIC TAGS: organoboron compouJ chloroborane, boron addition, diene boridation,
diallyl, pen ~ad-ie-ne-,-Vu-ta-d-i-en-e-,--'U6rocyclopentane
ABSTRACT: In order to determine the effect.of the nature of the diene on addition..
across the double'bond, the authors studied the addLtion of,chloroborane to dially~ -1
pentadien-1,4 and butadien-1,37in ether solutionat room temperatures, Chromato-
graphy and degradation of the-reaction products showed that diallyl adds primarily
in the 1,6 position (74%), with smaller amounts of 1,5 and-2,5 addition products..
Fractional distillation of this mixture resulted in good yields of pure 1-chloro-
borocyclopentane. Addition to pentadien-1,4 took.place in both the 1,5 and,1,4
positions (53% and 47%, respectively), while addition to butadien-1,3 was mostly
irk the 1,4 position (75%), with 21% of the 1,3 addition product. The reaction
conditions and yields are given. Orig. art. has: 2 chemical equations.
ASSOCIATION: Institut organicheskoy khimii im. N. D. Zelinskogo Akademii nauk
Card 1/2
ACCESSIC~- NR: A.P403-3385 s/oo62/64/ooo/oo4/o632/o637
11=1 i. Sheludyakov, V. D.; Shchc,~oleva, T. A.; MiJkhaylov, B. M.
-2T'71T~7: Or~~Lnic boron comDounds.
1_1 11 -
Co=-unication 129. reaction of alky1mercaptoborane trimers vith primary aminea.
SOIL-7RCE: All SSSO.R. Izvestiya. Scriya Idaimicbesk'aya, no. 4, 1964, 632-0537
TOPIC TtiGS: or_.zanic bo-ron compound, al-ky1mercaptoborane trimer, all-,11mercepto-
boranc triz:cr ariine reaction, reaction mechaniam, me-thylamine ziethyl-
=ercaptoboro-ne complex, borone chloride
ABS"Tit.-IO-P, The reaction of al~~lmerca_-Dtoborane trimers with primary amines was
studiea. Action of methylamine on methyLTaercaptolborane gives the riat-yl mercaptide
U
of bis(methyL~;mine)borone regardless of the reagent ration (trimer:arr--'-ne of 1:6 or
1:3). The mechanism suggested is the fozz=ation of an intermediatc n,-,atral complex,
r,ethylamine-methylmercaptoborane, which reacts more rapidly with -nethylamine than
the trii-,er. The le6s stable ethylmercaptide of bis(ethyl=1ne)borone is formed
similarly. These compounds exchange the mercitide ion for the chloride ion under
action of ether solut Ions or HCJ: fH 2B(NH2R' 2-,7SR+ HC1 -EE2B(N'L,2R)2-7C' +
.Car-4 1/2
ACCESSION, Nil: AP4033385
RSH. Similar exchange is effected ~writh benzyl chloride. Normal-butylamine Will
not fom the corresponding ethylmercaptide bis(n-butylarnine)borone, only the
c0m-Plex C21'5 SBH2 N"2C4H This vill react with benzyl chloride to form the salt
L- H2B(Iffl C 11 ) jC1. throne salts vith other amines in the capacity of addends
.were sQi~r~y ~;rmed by treating alkylmereaptoboranes with mixtures of the amine
:and benzyl chloride. The chlorides of bis(propyl, isopropyl, isobutyl, t-butyl,
~n-amyl, n-hexyl, or benzyl)borones are crystalline, stable, ether-insoluble
.materials. Orig. art. has: 2 tables and 12 equations.
ASSOCIATIO.N: Institut organicheskoy khimii im. N. D. Zelinskogo AkademJJ nauk
ESSR (Institute of Organic Chemistry, Academy of Sciences,SSSR)
SMUTMD: 3lOct63
SUB CODE; OC
C --- ~ :2/2
a rd, .
ENCL: 00
NO FT-X- SOV. 002 OTHER: 001
Abstiacts Under the action "of (fi-methilamino'o'n',b4roIL-tr-3*L-~hloride and
)boron tribromide in a 2s1 reagent ratio, dichloro-bia(dimethylamine)--
'boronium chloride and di~brotao-bia(dimethylamine)boronium bromide are
,formed, respectivel . The SaMO*Salta are, roduced by thereaction of
P
"dimethylaminoboron dihr-l idea. With dimethylammouium salts. A boronium
.Balt containing two different amines in the inner sphere, dichloro-:~~
'dimethylaminepyridineboroniixm chloride, vas synthesized bjr theaction
!of pyridine hydrochloride on dimethylaminoboron dichlori!12-1--aa well as
Card 1/2
ACCESSION NR: AP5015654
'the 'e~:ction - f bo. ri amino a.
'by r ). o ron trichlo ido,'-.pyridino, and dimethyl (in"
Jyhe
,1zl ratio a other and tetrahydrofuran solutions of boron trich-
~lqride were treated with ferric chlorideor stannic chloride, dichlcLro,-
.bia(dietboxide)boronium and dichioro-bia(tefrahydrofuran)-boronium
itetra-chloroferrates and dichloro-bia(-tetrahydrofuran)boronium hex&chloro--'.-,-.,-
:stannate were farmed, indicating that.in'other solutions boron trilii~fidai' _'1*1-
,exists not only in the form of.etherate: (BX3-0R2)) but.&ISO in the form.
tof cationic complexest in equilibrium v th the othoratos.;"6rig. arii. ha's 7-:
formulas.
ASSOCIATION: Institut organicheakoy-
khim,-i lm-~ N. D. ZeIiiiskogo Akademii nauk SSS,R -i-
(:Enstitut6 of Organic Ghemistry, Academy of Sciences, SSSR)-'
.qTMMTTTF,n! 71 Avah( *4 rKr.T. Ann MM. no P-"
7
DYAKOV, V,
Fart --c by,;!~ 7
Ai
bcron s-cipplexes. Zhu--r. cb, kh'in. -,5 no.EtIC66-1071
7~
(ICRA
, 11"
: "'A, , :".I. -ui Ye,N,~ KISEI-EV, V.G.-, MIKHAYLOV, B.M.
I,.- , r 'o vA " I
O-gan~,,bcrori :c~mrjunrfs. ;-,,ar*, 1q8.; Hydrclooration rf dienp-3 by
n- butylrrercap~,Oboranp, Zhur. ob. k~-'Tn. 35 no.6,dD78-1083
.Tf-, 165 . (MIRA 18:6)
I :i - . : I .
I I . ", I - - . I - I -. I . .I . o - ,
,-v
~ -; , -~ - . - -- -, - -a~ : 1.~I~ ~ ,, , .
: , . - - . ~ -, :-: , -.' - , - * -- I I . - . . . - ,
T
GLAZGVA, 0. 1., doktor med. nauk; lZRAELIT, S. S.; SHCHEGOLEU. ,
LEIN, B. N. - ------
Diagnosis of the active phase of the cardiac form of rheirratic
fever. Terap. arkh. no.12:30-35 161, (MIRA 15:2)
1. Iz teraperticheskoy kliniki (zav. - prof. P. L. Suk'~inin) i
laboratorii (zav. - kandidat meditsinskikh nauk V. V. Novosell-
skaya) Moskovskogo nauchno-issledovatellskogo instituta skoroy
pomoshchi imeni Sklifosovskogo.
(RHEUMATIC MART DISEASE)
~3 L-~ V.
126-5-3-31/31
T I I'LE. r-ns -A-E-e-i-l-S 1111o.-,- ~__--Zn.-Cu
U_
c a tr a v I n a v s t ar e.-;-a F~l -- e m s D 1 a -..re - Cu)
PEIPIO DI C A1. F il:_- Ll e_ t 1 o v i .-.1etallovedei, i'le, 19157, Vol
3,
AES __,1 C :-L" s C.'C. re For~-3 (_Ref,-~. ap, 2)
JTir,
DaL-1,_-era- in ~i_-,ystals of va-_,_-;ouE. suts-tances f-2:-e
.1 i11
-h:, :.urfac,,e cf cpiral and bo Tic..
u-
d i I 't Duri_-_-,,-- el..3ctroa I-licroscopic
_f -Z- ro J,_r1,- and
after -,rel_4_;ina:_1,
spiral et-chin- z) a t t e r o f c
o-, ~'n;~ -U.-~ -Ile
U__
After -oars a in," o to, -a
d4 c] -ai- i-sult
4 4
In 1L r
-1 i- ve 1~iar'e cleans
b-_5~~ht cc-u-1J., be 53e-_~n at thc ste-os of 'a-he -u chin:--
F 1 2) ich corres-onided U'-o th zo s
or -to -IL-.he u of th-e separ
f par4- jC le S 7UinC
C i-I a s ~-he obLz~ri-' s-~~irals cc-aidi- be
v 11 a szin~sl- -ur:7--ers vector, On ulle
basis of U',e featul,es of the tec1inique of oadde L-_1pr_i:,1-U_-
Q
vial r-o--l~-d in :-he ~;iven case it crnr be asou-med
Card 1/7, '1 2
t~,=Ll th~~ etc-1--ir, stepC c:3-1- be deLe-ou-ed by m_aalnE of an
126-5-_-'-31/31
La:_-,ire of E'chin - Patterns i-n j-r: A~~e~n Allo- ~ Al-Zn-Cu
el~,ctron r,,iicr~,copa ualv for the viral diLslocatio-
-for a Bur-,--,.ers vector of at least 15-1210 I_rl reality
t~~t' Bur 21!` ill U!-~c 6iven case 'U'101,111i;, to several
"Ujldred,,- of AriE;_-'U-ro1L! This follows frord the analysiS
of spectroscopic exposures as ~,*:ell as from the fact
fliLiL "Ae'Ps Z~I- clearl-v visible fro:a "he o-,-ide i-m-Prints,
It be concluded ~h,_,..t each etchinj7 pattern
is linked -DrotrLidin- to the curface of the alloy
of sovo_-al larL~er or gii~antic spiral dislocations zhich
are pa_-_--~liei to the cuIoic axes of ti-te crystal. (In, vievr
cf t-ho fact t.11'at, Bo-at-_!ue_',,, .V. (Ref -5) detected llelinoidal
,~i-locatior_c in- CaFq, the pos.,ibJlit-,, arose to associate
e~c~dnc--,- -L)at-L6~rlls helinoidal and prismat4c
oi-) U-,.-all-y in the centre of each T)hase of
patte-r-n -not one but-, several (mostly three)
S,--iral disloc~:!tioriz of a Sin-le siGn will occur. However,
L)
L, ne coi-,-le-xity of soille of the cpirai etchin- patterns
T" U -
load's to -~h- as:,;iuaptior, that in a number of cases
disloc-a-'~-Iions of C,-,)nosite sLns tal-e place at the face
centrec. Thus ) contrary to existinG theoretical
concen (T
Card 2/3 Ref.2.) on the effect that it is not justified
126-5-3--31/31
811 AgeinZ Alloy 1-Zn-Cu
A
L.LsL~-;(J -Orcsen-e of major disloc--tions _Lr_ _-.etals,
the cf detected
_onsjl-i Bur-ers vectors of seyreral
detected earlier in metals only
11, R e f a nd Steinber;-- (Ref.4). Ame 1i nx
Olb_-_--i-,~,_~ 115 :D--- crl-Etals Fsrow-n by depositirL~_- -,old
Zclul.-_ion of _--ea~:aiaatio= of YaCl; Steinberj,-,
it on -11-itaniuir, cr-,7stalc produced e le ctro lytic ally,
In bc-~-11 caf~es the ar-)(,_ar_,nce of --isantic
,!_!2)nca4-'-_ions caT, be caused by the pertainiL-L; spccific
f'01, in_~tance -rowth on foreirni body crystals.
-c-inted cut ~L_,'t in hic- "old
c r'~ 41-als c6ulJ c-itliel, follow the spircl di_-1o:-,-',.tiorLs of
-.11t or aol)ear due to major ron-corres--D:)ndence
of crystall c;f' -old and MaCl. In ~tt'e
01__Oar11.'.'iO.11'~E such conditions have appa,-ren-;ly
been made impossible.
Card 3/3 There are 2 fi._-ures and 5 references, 1 of which is
Soviet, 11,
11ote: This is a co--i-Dlete -translation.
ASSOCIATIOT~: I1!Sti-Ut fi7il7i Taetallov Uralls!_-_o~;o filiala AN SSSR
(Institute of Metal Physics, Ural Branch of the Ac.Sc.USSRL)
SUB.MITTED: April 11, 5 7
1. Allirdnur-copper--~ine alloys--Aging 2. Aluminuirr-copper-zine alloys
--Crystal struclLxe 3, Crystais-r'Physical properties
66227
SOV/126-6-3-10/33
AUTHORS: Buynov, N.N., Shchegoleva, T.V., Rakin, V.G.,
Komarova, M.F, and Zakharova, R.R.
PITLE: Electron Microscopic Investigation of Etca Figures in
Age Hardening Aluminium Alloys
.rE,110DICAL: Fizika metallov i metallovedeniye, 1959, Vol (6, Nr 3..
PP 367-393 (USSR)
40STRACT: The results of an electron microscopic investigation
of dimensions, form and structure of etc"x figures in
age hardening aluminium alloys are discussed. 11.1 tile
table on p 388, data of the dimensions and shape of tiie
etch figures for various alloys are given. The
dimensions of the figures change within very wide iimits
from several microns to a few tenths. It is
characteristic that for the majority at' quenched, sli,rhti-,
aged specimens the etch figures are straight-sided (F-Lg 1)
and fox- the haz~dened alloys they have an oval shape
(Fig 2). Their dimensions decrease in relation to time
and artificial ageing, when the hardness of tiie alloys
increases. In Fig 3, an electron micrograpil of an
Al-Zn-Cu (101/,0' Zn and 0.55/0' CU) alloy, deformed by
Card 1/2 compression by 1550' and aged at 180 C for b hours, is shown
66227
SOV/126-6-3-16/33
E'lectron Microscopic Investigation of Etch Figures in Age Hardei-Liar,
A.J'Aw.inium Alloys
Spiral steps can be seen. Fig 4 is all electron
micrograph of an Al-Cu (4% Cu) alloy aSed at 22C 0C f or
5 Inin. Craters can be seen at the to,i of octahedra,
suggesting screw dislocations. Fig j stiows sc~iewe for Lae
layout of 1,rimary mosaic blocks in the cry6tallinc ailoy;
tile 1.ossible axes along which new blocks can Lorizi are
shown by arrows. The authors arrive at tile following
conclusions: (1) The shape and dimensions of etc.i
figures in aluminium alloys change with tiie time and
temPerature of ageing. (2) The relation~5.aip between etci,
figures and large screw or spiral disiocations justifi--3s
the as-stii-ption that they correspond to mosaic i~--Iocks,
T;iere are j figures, 1 table and 17 refereAces, 7 Oi W.LiCh
re Soviet, 1 German, 1 Dutch and 6 ..n.,
C
ASSQ~CIAT!ON:Institut fiziki metallov AN SSSR (Institute of Y-e-cal
Physics AS USSR)
SUBMITTED: August 19-, 1958
Card 2/2
SOV/126-8-3-21/33
AUTHORS: Buynov, N.N. and Shchagoleva, T.V.
TITLE: A Few Characteris,~ics of the Distribution of Etch
Figures in an Al-Zn-Cu Alloy
PERIODICAL:Fizika metallov i metallovedeniye, 1959, Vol 8, Nr 3,
pp 455-457 (USSR)
ABSTRACT: on studying the electrolytically polished and chemically
etched (aqua regia) surface of an Al-Zn-Cu alloy
(10% Zn, 0.5% Cu) which had been deformed in
compression by less than 11%, spirals were observed
which may possibly illustrate either Frank and Read's
mechanism (Ref 1) or the existence of screw or helical
dislocations. Beside them loops were observed, which
were similar in shape to dislocation loops emitted by
Frank and Read sources. They were observed not only
within the grains (Fig I and 2) but also in grain
boundaries (Fig 3). In the first case they are met with
more frequently in groups, each of which contain from
2 to 7 loops. In those cases where the loops are not
continuous, they have the shape of hooks, the ends of
which are bent inwards (Fig I to 6), which points to
Card 1/2 their non-accidental origin. Light photographs in a
SOV/126-8-3-21/33
A Few Characteristics of the Distribution of Etch Figures in an
AI-Zn-Cu Alloy
dark background (Fig 3) show that the loops consist of
etched figures. However, there is one characteristic in
the distribution of the loops which makes it doubtful
as to waether they were formed due to the work of Frank
and Read sources. In the central portion of several
loop groups, a few small hooks with different
orientation are observed in each group (in Fig 1 shown
by an arrow). This peculiarity is difficult to
understand if one takes Frank and Read's dislocation
propagation as a basis and the authors of this paper
have come to the conclusion that these loops are due to
local stresses in various portions of the alloy.
Gratitude is expressed to A.N.Orlov for discussion of
the results of this paper. There are 6 figures and
4 references, 2 of which are Soviet and 2 English.
ASSOCIATlGtN:Institut fiziki metallov AN SSR (Institute c;f Metal
1hysics AS USSR)
SUBMITTED: August 12, 1950"
Card 2/2
69696
S/126/60/009/03/019/033
E091/E435
AUTHORS: Lerinman, R.M., Shchegoleva, T.V., Kushakevich, S.A.
and Selitskaya,
TITLE: Electron Microscopic Investigation of Structural
1~ Transformations in Titaniuai3Manxaneseyland Titanium-
-~Chromium Alloys
V
PERIODICAL:Fizika metallov i metallovedeniye, 1960, Vol 99 Nr 3,
PP 437-440 (USSR)
ABSTRACT% The transformation of the P-phase on tempering quenched
Ti--Mn and Ti-Cr alloys were studied. The following binary
alloys, containing elements which stabilize the P-phase,
were used for the investigationg Ti-Mn (10.5% Mn) and
Ti-Cr (9.4% Cr). The alloys were prepared from titanium
sponge of TGO quality, manganese of MR1 and chromium of
KhO quality. Ingots were prepared by double vacuum melting.
For the alloy containing Mn, the second fusion was carried
out in argon. The composition of the alloys is shown in
the table on p 438~ The ingots were deformed by hot
rolling and forging and the alloys were water quenched
from 8~OOC (ie from the p-region). The time of heating
Card 1/3 prior to quenching was 30 minutes. Tempering was carried
V
69696
S/126/60/009/03/019/033
E091/E435
Electron Microscopic investigation of Structural Transformations
in Titanium-Manganese and Titanium-Chromium Alloys
out by soaking for I to 25 hours at 400 to 550*C and
cooling in air. In order to reproduce the structures
of the alloys, single-stepped angular prints (replicas)
were prepared (Ref 10). The specimens were first
chemically polished in anhydrous boiling ortho-phosphoric
acid for 1 to 2 minutes. They were then etched in a
mixture of 20yo HF, 20% HN03 and 6o% glycerin.The etching
time varied from a few seconds to one minute. Apart
from the electron microscopic investigation, hardness
tests were made on a Rockwell machine with a diamond
indenter, using a load of 150 k9. In Fig la,lb and 1B,
the microstructures of specimens of Ti-10.5%Mn alloys
as tempered at 4000C for 1, 5 and 25 hours, respectively,
are shown; in Fig 1g, 1d and le, those of similar
specimens tempered at 550QC for 1, 10 and 25 hours,
respectively. Fig 2 shows the microstructure of a
Ti-9.4% Cr alloy (a - after quenching and tempering at
4000C for one hour; b - after quenching and tempering
Card 2/3 at 500'C for 25 hours). From the above microstructures
696~6
S/126/60/009/03/019/033
E091/E435
Electron Microscopic Investigation of Structural Transformations
in Titanium-Manganese and Titanium-Chromium Alloys
it can be seen that an w-phase appears in Ti-Cr and
Ti-Mn alloys after quenching and tempering at 4000C.
It has the shape of very finely dispersed platelets,
300-400 A thick. Periodically, chains of equiaxed
particles and individual equiaxed particles can be
observed which point to the fact that the w-phase nas
an equiaxed shape from the very moment of its formation.
Gratitude is expressed to Yu.A.Bagaryatskiy and
V.I.Dobatkin for the discussion of the results of this
work. There are 2 figures, I table and 10 references,
7 of which are English, 2 French and I Soviet.
ASSOCIATION:Institut fiziki metallov AN SSSR
(Institute of Physics of' Metals AS USSR)
SUBMITTED: April 22, 1959
Card 3/3
Sj' HKiLLVA, T..-A,, 6ffi-,LUDYA---'U-V
J., A
ijok
DO 3 ?
()Y D,Z=l!nslro,o
(Metal, icjjs)
LERBIMAN, H...M.., Sik;HEG~~!,E.VA, T,V.; PAVLOVA, (;.V,; ADOLINIA, T.I.
Elur.,tron micro.,3copy of* plnqfl.,~ dt!l',jrm,it!Dn:3 in
,,jLloys. Fiz. mot. I metallr)v,!ri. H rio.4:6231-630 0 '64, ;'PIRA IF:4)
1. Instittit fiziki metallov AN 3SSR.
GRANDBERG, I.I.; DIN VLY-FY; SHICHEGOIZIVAI V.I.; KOST, A.N.
pyrazoles. Part 18. Dehydrogenation of 3-hydroxy- and 3-amino-
pyrazolines with sulfur. Zhur.ob.khim. 31 no.6:1892-1896 Je 161.
UMiL 14:6)
1. Moskovskiy gosudarstvennyy universitet.
(Pyrazoline) (Dehydrogenation)