HRID1679933

反应详情

EQUATION

反应方程式

HRID 1679933 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.0 g (29.8 millimoles) of 2-(p-aminophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one, 4.2 g (35.4 millimoles) of 1-methylcyclopropanecarboxylic acid chloride and 150 ml of absolute tetrahydrofuran are refluxed for 7 hours. The product is filtered off at 10° C., washed with water and recrystallized twice from a dimethylformamide/water mixture. 4.5 g (53% of theory) of 2-[p-(1-methylcyclopropylcarbonylamino)-phenyl]-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one are obtained as pale beige crystals, of melting point 253°-255° C.

WORKUP

后处理

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