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RU2218341C2 - Method for preparing 1-ethyl-2-aza-3-methyl-4- alkylidenealumacyclohept-2-enes - Google Patents

Method for preparing 1-ethyl-2-aza-3-methyl-4- alkylidenealumacyclohept-2-enes Download PDF

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RU2218341C2
RU2218341C2 RU2002103992/04A RU2002103992A RU2218341C2 RU 2218341 C2 RU2218341 C2 RU 2218341C2 RU 2002103992/04 A RU2002103992/04 A RU 2002103992/04A RU 2002103992 A RU2002103992 A RU 2002103992A RU 2218341 C2 RU2218341 C2 RU 2218341C2
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preparing
aza
ethyl
methyl
alkylidenealumacyclohept
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RU2002103992/04A
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RU2002103992A (en
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У.М. Джемилев
А.Г. Ибрагимов
Л.О. Хафизова
Г.Н. Гильфанова
А.З. Шарипова
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ГУ Институт нефтехимии и катализа АН РБ и УНЦ РАН
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Abstract

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to method for preparing aluminum-organic compound that can be used in fine organic and organometallic synthesis. Invention describes method for preparing 1-ethyl-2-aza-3- methyl-4-alkylidenealumacyclohept-2-ene by interaction of terminal allene with triethylaluminium in the presence of catalyst Cp2ZrCl2 in argon atmosphere under normal conditions in methylene chloride for 5 h and the following addition of acetonitrile to reaction mass and stirring for 4-8 h at temperature ~40 C. Method provides preparing new compound with high regioselectivity and yield of the end product up to 42-58%. EFFECT: improved preparing method. 1 tbl

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Текст описания в факсимильном виде (см. графическую часть). Description text in facsimile form (see graphic part).

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Способ получения 1-этил-2-аза-3-метил-4-алкилиденалюмациклогепт-2-енов общей формулыThe method of obtaining 1-ethyl-2-aza-3-methyl-4-alkylidenealuminocyclohept-2-enes of the General formula
Figure 00000005
Figure 00000005
 где R = н-С6Н13, н-С8Н17,where R = n-C 6 H 13 , n-C 8 H 17 , характеризующийся тем, что терминальные аллены общей формулыcharacterized in that the terminal allens of the general formula R1-CH=C=CH2,R 1 —CH = C = CH 2 , где R1 = н-С6Н13, н-С8Н17,where R 1 = n-C 6 H 13 , n-C 8 H 17 , взаимодействуют с триэтилалюминием (AlEt3) в соотношении R1-CH=C=CH2: AlEt3 = 10:10-14 ммоль в присутствии катализатора цирконацендихлорида (Cp2ZrCl2), взятого в количестве 0,2-0,6 ммоль, в атмосфере аргона при комнатной температуре и атмосферном давлении в хлористом метилене в качестве растворителя в течение 5 ч с последующим добавлением к реакционной массе ацетонитрила (CH3CN), взятого в 3-кратном избытке по отношению к триэтилалюминию AlEt3, и перемешиванием реакционной массы в течение 4-8 ч при температуре около 40°С.interact with triethylaluminium (AlEt 3 ) in the ratio R 1 -CH = C = CH 2 : AlEt 3 = 10: 10-14 mmol in the presence of a catalyst of zirconacenedichloride (Cp 2 ZrCl 2 ), taken in an amount of 0.2-0.6 mmol in an argon atmosphere at room temperature and atmospheric pressure in methylene chloride as a solvent for 5 hours, followed by the addition of acetonitrile (CH 3 CN), taken in a 3-fold excess with respect to triethylaluminum AlEt 3 , to the reaction mass and stirring the reaction mass for 4-8 hours at a temperature of about 40 ° C.
RU2002103992/04A 2002-02-12 2002-02-12 Method for preparing 1-ethyl-2-aza-3-methyl-4- alkylidenealumacyclohept-2-enes RU2218341C2 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5030741A (en) * 1988-05-19 1991-07-09 Merck Patent Gesellschaft Mit Beschrankter Haftung Cyclic organometallic compounds
RU2139876C1 (en) * 1998-02-12 1999-10-20 Институт нефтехимии и катализа с опытным заводом АН Республики Башкортостан Method of obtaining of 1-(dialkylamine)-3-alkylalumacyclopentanes

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5030741A (en) * 1988-05-19 1991-07-09 Merck Patent Gesellschaft Mit Beschrankter Haftung Cyclic organometallic compounds
RU2139876C1 (en) * 1998-02-12 1999-10-20 Институт нефтехимии и катализа с опытным заводом АН Республики Башкортостан Method of obtaining of 1-(dialkylamine)-3-alkylalumacyclopentanes

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ЗАХАРКИН Л.И. и др. Синтез некоторых циклических алкилалюминийоксидов и алкилалюминийамидов. Изв. АН СССР, ОХП. - 1962, №5, с. 824-827. *

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