HRID660847

反应详情

EQUATION

反应方程式

HRID 660847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14.65 g (57.7 mmol) of 2-(4-chlorobenzoyl)-N-cyclopropylhydrazinecarboxamide from Example 2A are heated under reflux overnight in 60 ml 2 N aqueous sodium hydroxide. After cooling, the mixture is acidified to pH 1 with 2 N hydrochloric acid and extracted with ethyl acetate. The organic phase is dried over sodium sulphate, filtered and concentrated. The residue is stirred with dichloromethane, and the resulting precipitate filtered off, then washed with dichloromethane and dried in vacuo. 10.9 g (69% of theory) of the target compound are thus obtained.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phase is dried over sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. filtrationthe resulting precipitate filtered off
  7. washwashed with dichloromethane
  8. customdried in vacuo
  9. custom10.9 g (69% of theory) of the target compound are thus obtained