HRID1679935

反应详情

EQUATION

反应方程式

HRID 1679935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.0 g (24.8 millimoles) of 2-(p-aminophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one, 5.2 g (30.0 millimoles) of 2,2-dichlorocyclopropanecarboxylic acid chloride and 100 ml of absolute tetrahydrofuran are refluxed for 6 hours. The product is filtered off at 10° C., washed with water and recrystallized from a dimethylformamide/water mixture. 4.1 g (49% of theory) of 2-[p-(2,2-dichlorocyclopropylcarbonylamino)-phenyl]-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one are obtained as colorless crystals, of melting point 264°-265° C.

WORKUP

后处理

  1. filtrationThe product is filtered off at 10° C.
  2. washwashed with water
  3. customrecrystallized from a dimethylformamide/water mixture