HRID1378048

反应详情

EQUATION

反应方程式

HRID 1378048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.17 g (15 mmol) of crude 3-(3-aminomethyl-1,2,4-oxadiazol-5-yl)-7-chloro-5,6-dihydro-5-methyl-4H-imidazo[1,5-a][1,4]benzodiazepin-6-one, 45 ml of N,N-dimethylformamide, 6.5 ml (37.5 mmol) of N-ethyldiisopropylamine and 3.63 g (30 mmol) of allyl bromide were stirred at room temperature for 1 hour. The reaction solution was evaporated and the residue was chromatographed on 250 g of silica gel while eluting with ethyl acetate. The uniform fractions having the larger Rf value were evaporated. There were obtained 4.84 g (76%) of 3-(3-diallylaminomethyl-1,2,4-oxadiazol-5-yl)-7-chloro-5,6-dihydro-5-methyl-4H-imidazo[1,5-a]-[1,4]benzodiazepin-6-one, which was converted into the hydrochloride of m.p. 125°-130°.

WORKUP

后处理

  1. customThe reaction solution was evaporated
  2. customthe residue was chromatographed on 250 g of silica gel
  3. washwhile eluting with ethyl acetate
  4. customwere evaporated