HRID1658532

反应详情

EQUATION

反应方程式

HRID 1658532 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.1 ml of methyl isocyanate is added to a suspension of 5 g of 2-hydrazino-5-o-chlorophenyl-7-ethyl-3H-thieno[ 2,3-e] [1,4] diazepine in 100 ml of tetrahydrofuran, and the resulting mixture is stirred at room temperature for 2 hours. Then the reaction mixture is poured into ice water, and the precipitated crystals are collected by filtration, washed with water, dried, and recrystallized from a mixture of chloroform and ligroin to give 2-(4-methylsemicarbazido)-5-o-chlorophenyl-7-ethyl-3H-thieno[ 2,3-e][1,4]diazepine, melting at 213°-215° C.

WORKUP

后处理

  1. filtrationthe precipitated crystals are collected by filtration
  2. washwashed with water
  3. customdried
  4. customrecrystallized from a mixture of chloroform and ligroin