SU513962A1 - The method of obtaining indacene or its methyl derivatives - Google Patents
The method of obtaining indacene or its methyl derivativesInfo
- Publication number
- SU513962A1 SU513962A1 SU2046213A SU2046213A SU513962A1 SU 513962 A1 SU513962 A1 SU 513962A1 SU 2046213 A SU2046213 A SU 2046213A SU 2046213 A SU2046213 A SU 2046213A SU 513962 A1 SU513962 A1 SU 513962A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- indacene
- obtaining
- methyl derivatives
- yield
- reaction
- Prior art date
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Пример 1. В круглодонную колбу, снабженную механической мешалкой и обратным холодильником, помещают 65 г (0,5 мол ) пдивинилбензола 200 г 30--32%-ного водного раствора формальдегида (2 мол ) и 15 г катионообменной смолы КУ-2 (СОЕ 4,95 мг-экв/г; влажность 23,4). Реакцию ведут при интенсивном перемешивании при 80- 100°С в течение 3,5 ч. Обработка продуктов реакции включает отделение органического сло от водного промывку водного сло эфиром , объединение эфирных выт жек с органическими продуктами реакции, удаление неирореагировавшего формальдегида с иомош,ыо водного раствора аммиака и разгонку.Example 1. In a round bottom flask equipped with a mechanical stirrer and reflux condenser, 65 g (0.5 mol) pdivinylbenzene 200 g of 30–32% aqueous formaldehyde solution (2 mol) and 15 g of cation exchange resin KU-2 (SOY 4.95 mEq / g; moisture 23.4). The reaction is carried out with vigorous stirring at 80-100 ° C for 3.5 hours. Treatment of the reaction products involves separating the organic layer from the aqueous washing of the aqueous layer with ether, combining the ether extracts with the organic reaction products, removing un-reacted formaldehyde from the aqueous solution. ammonia and distillation.
В результате получают 92,0 г вещества 1а (Т. кип. 218°С) 2 мм рт. ст., выход 73,6%).The result is 92.0 g of the substance 1a (T. kip. 218 ° C) 2 mm Hg. Art., yield 73.6%).
25 г (0,1 мол ) 1а пропускают с объемной скоростью 0,7-1,5 ч в смеси с вод ным паром при температуре 380°С через кварцевую трубку, заполненную кальций-фосфатным25 g (0.1 mol) of 1a are passed at a bulk velocity of 0.7-1.5 h mixed with water vapor at a temperature of 380 ° С through a quartz tube filled with calcium phosphate
катализатором КДВ-15. После охлаждени продуктов реакции, отделени водного сло , получают 12,2 г Па (Т. пл. 67°С, выход 79,2%).catalyst KDV-15. After cooling the reaction products, separating the aqueous layer, 12.2 g of Pa are obtained (mp. 67 ° C, yield 79.2%).
Пример 2. В автоклав, снабженный механической мешалкой, загружают 65 г (5 молей) дивинилбензола, 88 г (2 мол ) уксусного альдегида и 15 ч катионита КУ-2 (СОЕ 4,95 мг-экв/г; влажность 23,4%). РеакциюExample 2. In an autoclave equipped with a mechanical stirrer, load 65 g (5 moles) of divinylbenzene, 88 g (2 moles) of acetic aldehyde and 15 hours of cation exchanger KU-2 (СОЕ 4.95 mg-eq / g; humidity 23.4% ). Reaction
провод т при температуре 90-95°С и интенсивном перемешивании в течение 8-10 ч. Обокончании реакции суд т по падению давлени в системе. Обработку продуктов реакции провод т по методике, описанной в примереcarried out at a temperature of 90-95 ° C and vigorous stirring for 8-10 hours. The termination of the reaction is judged by the pressure drop in the system. The treatment of the reaction products is carried out according to the procedure described in the example.
I, и получают 38,5 г 16 (Т. кип. 226°С/2 ммI, and receive 38.5 g 16 (T. Kip. 226 ° C / 2 mm
рт. т., выход 66,8%). При расщеплении 16 вHg t., yield 66.8%). When splitting 16 in
услови х, описанных в примере 1, получаютthe conditions described in example 1 are obtained
14,6 г II б (выход 80,0%, Т. пл. 64°).14.6 g II b (yield 80.0%, mp. 64 °).
Пиже приведены молекул рные массы иMolecular weights are shown below.
характеристические частоты полос поглощени в ИК-спектре соединений I и П.characteristic frequencies of absorption bands in the IR spectrum of compounds I and P.
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU2046213A SU513962A1 (en) | 1974-07-18 | 1974-07-18 | The method of obtaining indacene or its methyl derivatives |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU2046213A SU513962A1 (en) | 1974-07-18 | 1974-07-18 | The method of obtaining indacene or its methyl derivatives |
Publications (1)
Publication Number | Publication Date |
---|---|
SU513962A1 true SU513962A1 (en) | 1976-05-15 |
Family
ID=20591737
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
SU2046213A SU513962A1 (en) | 1974-07-18 | 1974-07-18 | The method of obtaining indacene or its methyl derivatives |
Country Status (1)
Country | Link |
---|---|
SU (1) | SU513962A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4568782A (en) * | 1985-06-17 | 1986-02-04 | The Standard Oil Company | Preparation of indenes |
-
1974
- 1974-07-18 SU SU2046213A patent/SU513962A1/en active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4568782A (en) * | 1985-06-17 | 1986-02-04 | The Standard Oil Company | Preparation of indenes |
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