HRID1418960

反应详情

EQUATION

反应方程式

HRID 1418960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stream of hydrogen sulphide was conducted for 1/2 hr. through a solution of 3.0 g (0.0103 mol) of 7-chloro-8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carbonitrile in 10 ml of pyridine and 1.0 ml of triethylamine. The green solution was left to stand for 64 hrs., then degassed with a stream of nitrogen and subsequently completely freed from the solvents. The residue was partitioned between dichloromethane and water and the suspension obtained was suction filtered. There were obtained 2.45 g (73%) of 7-chloro-8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]-benzodiazepine-3-thiocarboxamide.

WORKUP

后处理

  1. waitThe green solution was left
  2. custom, then degassed with a stream of nitrogen
  3. customThe residue was partitioned between dichloromethane and water
  4. customthe suspension obtained
  5. filtrationfiltered