RU2008132386A - METHOD FOR PRODUCING 2-ALKYL-5,6,7,8,9,10-HEXAHYDRO-4H-CYCLONONE [b] SELENOPHENES - Google Patents
METHOD FOR PRODUCING 2-ALKYL-5,6,7,8,9,10-HEXAHYDRO-4H-CYCLONONE [b] SELENOPHENES Download PDFInfo
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- RU2008132386A RU2008132386A RU2008132386/04A RU2008132386A RU2008132386A RU 2008132386 A RU2008132386 A RU 2008132386A RU 2008132386/04 A RU2008132386/04 A RU 2008132386/04A RU 2008132386 A RU2008132386 A RU 2008132386A RU 2008132386 A RU2008132386 A RU 2008132386A
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- diene
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- cyclonone
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- alka
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Abstract
Способ получения 2-алкил-5,6,7,8,9,10-гексагидро-4Н-цикжшона[b]-селенофенов общей формулы (1): ! ! характеризующийся тем, что смесь циклонона-1,2-диена и алка-1,2-диена (окта-1,2-диен, дека-1,2-диен, додека-1,2-диен) подвергают взаимодействию с этилмагнийбромидом (EtMgBr/эфир) в присутствии Mg (порошок) и катализатора титанацендихлорида (Cp2TiCl2), взятых в мольном соотношении циклонона-1,2-диен: алка-1,2-диен:EtMgBr:Mg:Cp2TiCl2=10:10:(22-26):20:(1.0-1.4), предпочтительно 10:10:24:20:1.2, в атмосфере аргона при комнатной температуре (20-22°С) и атмосферном давлении в течение 6-8 ч в диэтиловом эфире, с последующим добавлением эквимольного к EtMgBr количества селена (Se), бензола в качестве растворителя и нагреванием реакционной массы в течение 6 ч при температуре ~40°С, затем, после упаривания в вакууме легких растворителей, реакционную массу выдерживают 1 ч при температуре ~140°С.The method of obtaining 2-alkyl-5,6,7,8,9,10-hexahydro-4H-cycle of [b] -selenophenes of the general formula (1):! ! characterized in that a mixture of cyclonone-1,2-diene and alka-1,2-diene (octa-1,2-diene, deca-1,2-diene, dodeca-1,2-diene) is reacted with ethyl magnesium bromide ( EtMgBr / ether) in the presence of Mg (powder) and a catalyst of titanocene dichloride (Cp2TiCl2) taken in the molar ratio of cyclonone-1,2-diene: alka-1,2-diene: EtMgBr: Mg: Cp2TiCl2 = 10: 10: (22- 26): 20: (1.0-1.4), preferably 10: 10: 24: 20: 1.2, in an argon atmosphere at room temperature (20-22 ° C) and atmospheric pressure for 6-8 hours in diethyl ether, followed by adding equimolar to EtMgBr amount of selenium (Se), benzene as sol a specimen and heating the reaction mass for 6 h at a temperature of ~ 40 ° C, then, after evaporation of light solvents in a vacuum, the reaction mass is kept for 1 h at a temperature of ~ 140 ° C.
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Application Number | Priority Date | Filing Date | Title |
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RU2008132386/04A RU2389726C2 (en) | 2008-08-05 | 2008-08-05 | 2-ALKYL-5,6,7,8,9,10-HEXAHYDRO-4-CYCLONONE[b]SELENOPHENE SYNTHESIS METHOD |
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RU2008132386/04A RU2389726C2 (en) | 2008-08-05 | 2008-08-05 | 2-ALKYL-5,6,7,8,9,10-HEXAHYDRO-4-CYCLONONE[b]SELENOPHENE SYNTHESIS METHOD |
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RU2008132386A true RU2008132386A (en) | 2010-02-10 |
RU2389726C2 RU2389726C2 (en) | 2010-05-20 |
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RU2008132386/04A RU2389726C2 (en) | 2008-08-05 | 2008-08-05 | 2-ALKYL-5,6,7,8,9,10-HEXAHYDRO-4-CYCLONONE[b]SELENOPHENE SYNTHESIS METHOD |
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