HRID1606974

反应详情

EQUATION

反应方程式

HRID 1606974 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

3.73 g (10 mmol) of 7-chloro-4,5-dihydro-3-iodo-5-methyl-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one was stirred at room temperature for 20 hours with 1.12 g (11 mmol) of phenylacetylene, 70 mg of bis-(triphenylphosphine)-palladium(II) dichloride and 10 mg of copper(I) iodide in 20 ml of diethylamine. The reaction mixture was diluted with methylene chloride and washed twice with water. The organic phase was dried over magnesium sulphate and evaporated. After recrystallization of the residue from ethyl acetate there was obtained 7-chloro-4,5-dihydro-5-methyl-3-(phenylethynyl)-6H-imidazo[1,5-a][1,4]benzodiazepin-6-one of melting point 205°-206°.

WORKUP

后处理

  1. washwashed twice with water
  2. dry with materialThe organic phase was dried over magnesium sulphate
  3. customevaporated
  4. customAfter recrystallization of the residue from ethyl acetate