反应详情

A solution of 2.9 g (6.5 mmol) of N-(1-benzyloxycarbonylcyclopentyl)-N-(2'-cyano-biphenyl-4-ylmethyl)-amine hydrochloride and 4.4 ml (26 mmol) of Hunig base in 50 ml of ethyl acetate is treated with 1.1 g (9 mmol) of pentanoyl chloride, and the mixture is stirred for 15 hours at 25°-30°. After the addition of a further 0.5 g of pentanoyl chloride the mixture is stirred for a further 8 hours. The reaction mixture is then treated with 10 ml of aqueous ammonia solution (5%) and stirred for 0,5 hours. The ethyl acetate phase is separated, washed in succession with 2 N-hydrochloric acid, water and sodium hydrogencarbonate solution, dried and evaporated. The N-(1-benzyloxycarbonylcyclopentyl)-N-(2'-cyanobiphenyl-4-ylmethyl)-N-pentanoyl-amine is thus obtained in the form of a brown oil [Rf : 0.53 (system B7)], which is used for further reactions in crude form.

1. stirringis stirred for a further 8 hours
2. stirringstirred for 0,5 hours
3. customThe ethyl acetate phase is separated
4. washwashed in succession with 2 N-hydrochloric acid, water and sodium hydrogencarbonate solution
5. customdried
6. customevaporated