HRID660850

反应详情

EQUATION

反应方程式

HRID 660850 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.00 g (27.6 mmol) of 2-(2-chlorobenzoyl)-N-cyclopropylhydrazinecarboxamide from Example 10A are heated under reflux for about 60 hrs in 30 ml 3 N aqueous sodium hydroxide (conversion testing by LC/MS analysis). After cooling, it is acidified with 1 N hydrochloric acid and the mixture extracted three times with ethyl acetate. The combined organic phases are washed twice with saturated sodium hydrogen carbonate solution, dried over magnesium sulphate, filtered and concentrated. 3.32 g (48% of theory) of the target compound are thus obtained.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionthe mixture extracted three times with ethyl acetate
  3. washThe combined organic phases are washed twice with saturated sodium hydrogen carbonate solution
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custom3.32 g (48% of theory) of the target compound are thus obtained