HRID1638653

反应详情

EQUATION

反应方程式

HRID 1638653 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 2-amino-4,5-difluoro-3-methylthiomethylbenzonitrile (4.0 g) in ethanol (80 ml) are added Raney nickel (40 ml) with ethanol (80 ml). The mixture is stirred at 40°-50° C. for 30 minutes, and then filtered. To the filtrate is added water, the reaction mixture is extracted with ethyl acetate. The extract is dried over magnesium sulfate and concentrated. The product is recrystallized from n-hexane to give 2-amino-4,5-difluoro-3-methylbenzonitrile (2.4 g), as a white crystal, m.p. 114°-116° C.

WORKUP

后处理

  1. filtrationfiltered
  2. additionTo the filtrate is added water
  3. extractionthe reaction mixture is extracted with ethyl acetate
  4. dry with materialThe extract is dried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe product is recrystallized from n-hexane