SU479772A1 - The method of obtaining 2,3-bis- (o-carboranyl) -butadiene - Google Patents
The method of obtaining 2,3-bis- (o-carboranyl) -butadieneInfo
- Publication number
- SU479772A1 SU479772A1 SU1949903A SU1949903A SU479772A1 SU 479772 A1 SU479772 A1 SU 479772A1 SU 1949903 A SU1949903 A SU 1949903A SU 1949903 A SU1949903 A SU 1949903A SU 479772 A1 SU479772 A1 SU 479772A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- carboranyl
- butadiene
- bis
- obtaining
- product
- Prior art date
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
СиSi
НС-с гNS-with g
30-250С30-250С
о/about/
BjoHioBjohio
сн, /оmon, o
4. /С-СН4. / C-CH
с-with-
Выход целевого продукта 60%-80 7оПример . К амиду натри , полученному из 2,3 г Na (0,01 г же) в 300 мл аммиака, при -50° С добавл ют 9,9 г (0,03 моль) 1-(а,р-дибромэтил)-о-карборана в 50 мл абсолютного эфира и смесь перемешивают при (40) - (-60)° С 1,5 час. Затем большую часть аммиака испар ют при кипении и к остатку добавл ют воду. Водный слой экстрагируют эфиром и эфирные выт л ки сушат над хлористым кальцием. После отгонки растворител остаток кристаллизуют из гексана. Получают 5 г (67%) 1-(а-бромвинил)-о-карборана , т. ил. 60-6ГС.The yield of the target product 60% -80 7oExample. To sodium amide, prepared from 2.3 g of Na (0.01 g of the same) in 300 ml of ammonia, 9.9 g (0.03 mol) of 1- (a, p-dibromoethyl) - o-carboran in 50 ml of absolute ether and the mixture is stirred at (40) - (-60) ° C for 1.5 hours. Then most of the ammonia is evaporated at boiling and water is added to the residue. The aqueous layer is extracted with ether and the ether extracts are dried over calcium chloride. After distilling off the solvent, the residue is crystallized from hexane. 5 g (67%) of 1- (a-bromo-vinyl) -o-carboran, t. Il. 60-6GS.
Найдено, %: С 19,13; Н 5,16; В 43,46; Вг 31,53.Found,%: C 19.13; H 5.16; B 43.46; Br 31.53.
C4Hi3BioBr.C4Hi3BioBr.
,С 19,28; Н 5,26; В 43,49;, C 19.28; H 5.26; B 43.49;
Вычислено, Вг 32,08.Calculated, Br 32.08.
2600 (В-Н), 30802600 (B – H), 3080
- 1- one
ИК-спектр, IR spectrum
см ( С-Н), 1620 (С С).cm (C – H), 1620 (C C).
1-(а-бром7 ,5 г (0,03 моль) полученного экв) меди винил)-о-карборана и 3,2 г (0,05 г нагревают 8 час в пальчиковом автоклаве при 240-250° С. Продукт экстрагируют эфиром . После отгонки эфира остаток перекристаллизовьшают из гептана. Получают 2,5 г (50%) 2,3-бис-(о - карборанил) - бутадиена, т. пл. 304-306° С.1- (a-bromo, 5 g (0.03 mol) of the resulting eq) copper vinyl) -o-carboran and 3.2 g (0.05 g are heated for 8 hours in a finger autoclave at 240-250 ° C. The product is extracted ether. After the ether has been distilled off, the residue is recrystallized from heptane to give 2.5 g (50%) of 2,3-bis- (o-carboranyl) butadiene, mp 304-306 ° C.
Найдено, %: С 28,73; Н 8,25. Мол. вес (масс-спектрометрически) 340.Found,%: C 28.73; H 8.25. Mol weight (mass spectrometrically) 340.
СзНзбВгоВычислено , %: С 28,36; Н 7,75. Мол. вес. 338.SzNzbVgoCalculated,%: C 28.36; H 7.75. Mol weight. 338.
ИК-спектр, 2600 (В-Н), 3070 (С-Н), 1625 (С С-С С).IR Spectrum, 2600 (B – H), 3070 (C – H), 1625 (C C – C C).
Предмет изобретени Subject invention
1.Способ получени 2,3-б«с-(о-карборанил )-бутадиена, отличающийс тем, что1. A method for producing 2,3-b "c- (o-carboranyl) -butadiene, characterized in that
Claims (3)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU1949903A SU479772A1 (en) | 1973-07-19 | 1973-07-19 | The method of obtaining 2,3-bis- (o-carboranyl) -butadiene |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU1949903A SU479772A1 (en) | 1973-07-19 | 1973-07-19 | The method of obtaining 2,3-bis- (o-carboranyl) -butadiene |
Publications (1)
Publication Number | Publication Date |
---|---|
SU479772A1 true SU479772A1 (en) | 1975-08-05 |
Family
ID=20561731
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
SU1949903A SU479772A1 (en) | 1973-07-19 | 1973-07-19 | The method of obtaining 2,3-bis- (o-carboranyl) -butadiene |
Country Status (1)
Country | Link |
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SU (1) | SU479772A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1993008122A1 (en) * | 1991-10-23 | 1993-04-29 | Guerbet S.A. | Contrast agents and compositions for radiological imaging, and radiological imaging method utilizing same |
US5545397A (en) * | 1991-10-23 | 1996-08-13 | Boron Biologicals, Inc. | Contrast agents and compositions for radiological imaging, and radiological imaging method utilizing same |
-
1973
- 1973-07-19 SU SU1949903A patent/SU479772A1/en active
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1993008122A1 (en) * | 1991-10-23 | 1993-04-29 | Guerbet S.A. | Contrast agents and compositions for radiological imaging, and radiological imaging method utilizing same |
US5545397A (en) * | 1991-10-23 | 1996-08-13 | Boron Biologicals, Inc. | Contrast agents and compositions for radiological imaging, and radiological imaging method utilizing same |
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