HRID630423

反应详情

EQUATION

反应方程式

HRID 630423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-amino-2,5-difluorobenzoic acid (intermediate 137; 2.7 g; 0.015 mol) in hydrogen chloride 1.25 mL in ethanol (91 mL, 0.113 mol) was stirred for 24 hours at 60° C. The solvent was removed under reduced pressure and the crude obtained was treated with water and solid bicarbonate to obtain a basic pH, after few minutes stirring an extraction with ethyl acetate was done. The organic layer was washed with brine, dried and the solvent was removed under reduced pressure to give the title compound as a white solid (92%), which was used in the next step without further purification.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. customthe crude obtained
  3. customto obtain a basic pH
  4. extractionan extraction with ethyl acetate
  5. washThe organic layer was washed with brine
  6. customdried
  7. customthe solvent was removed under reduced pressure