HRID576877

反应详情

EQUATION

反应方程式

HRID 576877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of ethyl 2-(1-methyl-2-(benzylcarbamoyl)hydrazinyl)acetate (Compound XXXII-1) 1.33 g (5.0 mmol) in tetrahydrofuran/methanol/water (2:3:1) 24 ml, lithium hydroxide monohydrate 420 mg (10.0 mmol) was added and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with water 25 ml and washed with ether 25 ml. The aqueous phase was acidified with 10%-citric acid 25 ml and extracted with chloroform 30 ml. The organic phase was washed with brine 25 ml and dried with magnesium sulfate and then filtered. The filtrate was concentrated in vacuo to obtain the title compound 1.05 g (88%).

WORKUP

后处理

  1. washwashed with ether 25 ml
  2. extractionextracted with chloroform 30 ml
  3. washThe organic phase was washed with brine 25 ml
  4. dry with materialdried with magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated in vacuo