SU111490A2 - Method of stopping telomerization reaction - Google Patents
Method of stopping telomerization reactionInfo
- Publication number
- SU111490A2 SU111490A2 SU579625A SU579625A SU111490A2 SU 111490 A2 SU111490 A2 SU 111490A2 SU 579625 A SU579625 A SU 579625A SU 579625 A SU579625 A SU 579625A SU 111490 A2 SU111490 A2 SU 111490A2
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- solution
- methylene chloride
- added
- beats
- reaction
- Prior art date
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Предлагаемое изобретение вл етс распространением способа прекращени реакции теломеризации , инициируемой хлористым цин-ком , известного то.тько дл те.томеризации изопрена с хлористым прени .том, на реакцию теломеризации диеновых соединений вообще с хлоралкеиами . С целью образовани нужной цепи теломера, на опреде .ленной стадии процесса к реакционной смеси добавл ют аммиак или органическое основание (например, пиридин или диэтиламин).The present invention is a propagation of a method for terminating a telomerization reaction initiated by zinc chloride, known to be used for temperature testing of isoprene with chloride, on the reaction of telomerization of diene compounds in general with chloroalkenias. In order to form the desired telomere chain, ammonia or an organic base (for example, pyridine or diethylamine) is added to the reaction mixture at a certain stage of the process.
Пример. В раствор 52 г хлористого пренила и 26 с дивинила в 30 мл хлористого метилена с уд. в. 0,827 при минус 10 прибавл ют 2 мл 5%-ного раствора хлорного олова в хлористом метилене, смесь перемещивают до увеличени удельного веса на 0,094 и к ней добавл ют диэтиламин (гаситель).Example. In a solution of 52 g of prenyl chloride and 26 of divinyl in 30 ml of methylene chloride with beats. at. 0.827 at minus 10, 2 ml of a 5% solution of chlorine tin in methylene chloride is added, the mixture is moved until the specific gravity is increased by 0.094, and diethylamine (quencher) is added to it.
Раствор декантируют с осадка и подвергают разгонке.The solution is decanted from the precipitate and subjected to distillation.
Получают 71 г теломеров. из которых выдел ют 32 терпеновых х.юридов нзвестньпги приемами.71 g of telomeres are obtained. of which 32 are isolated, the terpeneic h.yrids are known.
П р и е р 2. В раствор 52 г 4-хлорпентена-2 и 34 г изопрена в 30 мл хлористого метилена с уд. в. 0,920 при прибавл ют 2 мл 5%-ного раствора хлорного олова в хлористом метилене, смесь перемещивают до увеличени уд. в. на 0,060 и к ней добавл ют диэтиламин .Example 2. To a solution of 52 g of 4-chloropentene-2 and 34 g of isoprene in 30 ml of methylene chloride with beats. at. 0.920 2 ml of a 5% solution of chlorine tin in methylene chloride was added, and the mixture was transferred to increase the beats. at. by 0.060 and diethylamine is added to it.
Раствор декантируют с осадка и подвергают разгонке.The solution is decanted from the precipitate and subjected to distillation.
Получают 43 г теломеров, из которых выдел ют 27 г терпеновых хлоридов.43 g of telomeres are obtained, of which 27 g of terpene chlorides are isolated.
П р и м е р 3. В раствор 52 с 4хлорпентена-2 и 26 г дивинила в 30 мл хлористого метилена с уд. в. 0,834 при минус 10 прибавл ют 3 мл 10%-ног() раствора хлорного олова в хлористом мети.тене, смесь перемеагивают до уве.шчепи уд. в. на 0,101 и прибавл ют диэтиламин.PRI me R 3. In solution 52 from 4 chloropentene-2 and 26 g of divinyl in 30 ml of methylene chloride with beats. at. 0.834 at minus 10, 3 ml of a 10% () solution of chlorine tin in methylene chloride is added, the mixture is reagentized to a maximum of 10 beats. at. by 0.101 and diethylamine was added.
Раствор декантируют с осадка и подвергают разгонке.The solution is decanted from the precipitate and subjected to distillation.
ГДшучаЯэт 80 теломеров, из коТ1эрых .в 1 §л Ют 52 t терпеповых хлоридов. 80 telomeres from among the cohorts. In 1 §l Yut 52 t terpovykh chlorides.
П р и .м ер 4. В раствор 52 ,- 4хлорпентена-2 и 34 г пиперклена в 30 мл хлористого метилена с уд. в. 0,904 при 10° добавл ют 2 M,I 5%-ного раствора хлорного олова в хлористом метилеие, смесЕз перемешивают до увеличени уд. в. на 0,044 и добавл ют диэтила.мин.P r and. M er 4. In a solution of 52, - 4 chloropentene-2 and 34 g of piperklena in 30 ml of methylene chloride with beats. at. 0.904 at 10 ° is added 2 M, I of a 5% aqueous solution of chlorine tin in methylene chloride, and the mixture is stirred to increase the beats. at. at 0.044 and diethyl is added.
Раствор декантируют с осадка и подвергают разгонке .The solution is decanted from the precipitate and subjected to distillation.
Получают 35 г теломеров, из которых выдел ют 27 г терненовых хлоридов.35 g of telomeres are obtained, of which 27 g of ternene chlorides are isolated.
Пример 5. В раствор 45 ,. хлористого кротила и 34 г изопрена в 50 мл хлористого метилена с уд. в. 0,976 при 17° добавл ют 2 г хлористого цинка в 4 мл метанола, смесь перемешивают до увеличени уд. в. на 0,058 и прибавл ют 3,5 мл пиридина.Example 5. In solution 45,. crotyl chloride and 34 g of isoprene in 50 ml of methylene chloride with beats. at. 0.976 at 17 °, 2 g of zinc chloride in 4 ml of methanol are added, and the mixture is stirred until the yield is increased. at. 0.058 and add 3.5 ml of pyridine.
Раствор декантируют с осадка и подвергают разгонке.The solution is decanted from the precipitate and subjected to distillation.
Получают 26 г теломеров, из которых выдел ют 15. терпеповых хлоридов.26 g of telomeres are obtained, of which 15. terpore chloride chlorides are isolated.
Пример 6. В раствор 43 г изопрена и 65 г его гидрохлорида-1,2Example 6. In a solution of 43 g of isoprene and 65 g of its hydrochloride-1,2
в 35 л;л хлористого мети.чена с уд. в. 0.903 при 17 добавл ют 1 мл 5%-ного раствора хлорного олова в хлористом метилене. Реакцию провод т при 2У до возрастани уд. в. на 0,03. Дл погашени реакции в реакционную смесь нропускают 40 мл газообразного аммиака.in 35 l; l of methylene chloride with beats. at. 0.903 at 17 was added 1 ml of a 5% solution of chlorine tin in methylene chloride. The reaction is carried out at 2U to increase beats. at. by 0.03. To quench the reaction, 40 ml of ammonia gas is dropped into the reaction mixture.
При разгонке по.тучают 28 с теломеров , из которых выдел ют 13,5 терпеновых хлоридов.In the course of distillation, 28 telomeres are extracted, of which 13.5 terpene chlorides are isolated.
Пример 7. В раствор 43 г изопрена , 65 г его гидрохлорида-1,2 в 35 мл хлористого метилена с уд. в. 0,901 при 17 добавл ют 1 мл 35%-ного раствора хлорного олова в хлористом метилене. Реакцию провод т до приращени удельного веса на 0,053. Погашают реакцию добавлением 0,13 г сухого карбоната аммони .Example 7. In a solution of 43 g of isoprene, 65 g of its hydrochloride-1.2 in 35 ml of methylene chloride with beats. at. 0.901 at 17 was added 1 ml of a 35% solution of chlorine tin in methylene chloride. The reaction is carried out until the specific weight is increased by 0.053. Quench the reaction by adding 0.13 g of dry ammonium carbonate.
При разгонке получают 34,5 s теломеров, из которых выдел ют 14 J терпеновых хлоридов.During distillation, 34.5 s of telomeres are obtained, of which 14 J terpene chlorides are isolated.
Пред м е Т и з о б р е т е н и PREFACE E and W obreteni
Применение способа нрекрашени реакции теломеризации но авт. св. 106808 дл непредельных соединений и галогенопроизводных, инициируемых катализаторами Фридел -Крафтса .Application of the method of dyeing telomerization but auth. St. 106808 for unsaturated compounds and halogen derivatives, initiated by Friedel-Crafts catalysts.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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SU579625A SU111490A2 (en) | 1957-06-27 | 1957-06-27 | Method of stopping telomerization reaction |
Applications Claiming Priority (1)
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SU579625A SU111490A2 (en) | 1957-06-27 | 1957-06-27 | Method of stopping telomerization reaction |
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SU106808 Addition |
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SU111490A2 true SU111490A2 (en) | 1957-11-30 |
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SU579625A SU111490A2 (en) | 1957-06-27 | 1957-06-27 | Method of stopping telomerization reaction |
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1957
- 1957-06-27 SU SU579625A patent/SU111490A2/en active
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