HRID1606039

反应详情

EQUATION

反应方程式

HRID 1606039 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[b] A mixture of 20 g of 5-o-chlorophenyl-7-ethyl-1,2-dihydro-3H-thieno[2,3-e][1,4]diazepine-2-thione and 9.6 g of aminoacetaldehyde diethylacetal is added to 200 ml of ethanol, and the whole mixture is refluxed for 2.5 hours. While the reaction mixture is hot, an activated carbon is added to the reaction mixture. The whole mixture is filtered and the filtrate is cooled. The crystals formed are collected by suction filtration and washed with a small amount of ethanol to give 23 g of 5-o-chlorophenyl-2-(2,2-diethoxyethylamino)-7-ethyl-3H-thieno[ 2,3-e][1,4]diazepine melting at 143° - 146°C.

WORKUP

后处理

  1. temperaturethe whole mixture is refluxed for 2.5 hours
  2. additionan activated carbon is added to the reaction mixture
  3. filtrationThe whole mixture is filtered
  4. temperaturethe filtrate is cooled
  5. customThe crystals formed
  6. filtrationare collected by suction filtration
  7. washwashed with a small amount of ethanol