HRID548774

反应详情

EQUATION

反应方程式

HRID 548774 的结构方程式

PROCEDURE

实验过程

A mixture solution of 14.5 mL (0.134 mol) of methyl acetoacetate and 20.2 g (0.134 mol) of cyclohexylhydrazine hydrochloride was stirred for 2 hours at 120° C., and the mixture was cooled. Then, the reaction mixture was neutralized with 30 mL of 4M-sodium hydroxide solution and extracted with ethyl acetate. The organic layer was washed with water and saturated saline solution and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the resulting residue was treated with hexane. The resulting precipitate was collected to give 19.0 g (79%) of the titled compound.

WORKUP

后处理

  1. temperaturethe mixture was cooled
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated saline solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. additionthe resulting residue was treated with hexane
  7. customThe resulting precipitate was collected