反应详情

Hexahydro-3-(3-methoxyphenyl)-2H-azepin-2-one (2.19 g) in dry tetrahydrofuran was added to a stirred solution of lithium diisopropylamide (from butyllithium 1.4 molar 15.7 ml, and diisopropylamine 3.15 ml) under nitrogen at 0° C. Ethyl bromide (1 ml) was added in one portion and the reaction allowed to warm up to room temperature. After two hours the reaction was poured into 2 M HCl, the organic layer separated and the aqueous layer extracted with chloroform. The combined organic layers were dried over magnesium sulphate, filtered and evaporated to an oil which was crystallised from ethyl acetate giving 1.68 g of the title compound m.p. 85°-7° C.

1. customthe organic layer separated
2. extractionthe aqueous layer extracted with chloroform
3. dry with materialThe combined organic layers were dried over magnesium sulphate
4. filtrationfiltered
5. customevaporated to an oil which
6. customwas crystallised from ethyl acetate giving 1.68 g of the title compound m.p. 85°-7° C.