HRID1679927

反应详情

EQUATION

反应方程式

HRID 1679927 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-(m-aminophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one (see Example 33), 3.5 g (44.6 millimoles) of acetyl chloride and 100 ml of anhydrous toluene are kept at 80° C. for 6 hours. The product is filtered off at 10° C., washed first with toluene and then with water, and recrystallized from methanol. 2.9 g (40% of theory) of 2-(m-acetylaminophenyl)-3,4-diaza-bicyclo[4.1.0]hept-2-en-5-one are obtained as almost colorless crystals, of melting point 200°-202° C.

WORKUP

后处理

  1. filtrationThe product is filtered off at 10° C.
  2. washwashed first with toluene
  3. customwith water, and recrystallized from methanol