HRID875392

反应详情

EQUATION

反应方程式

HRID 875392 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 3,5-difluoro-4-formylbenzonitrile (0.2 g, 1.1 mmol) in dimethylsulfoxide (10 mL), were added a aqueous solution of potassium dihydrogen phosphate (0.41 g, 2.9 mmol in 0.4 mL of water), sodium chlorite (0.216 g, 2.3 mmol in 4 mL of water) in one lot at an ambient temperature. The resulting reaction mixture was stirred for about 1 hour. The reaction mass was diluted with water (100 mL). The aquoeus phase was extracted with ethyl acetate (3×100 mL). The combined organic layer dried over anhydrous sodium sulfate, filtered and concentrated to afford 4-cyano-2,6-difluorobenzoic acid (200 mg, 91.32%).

WORKUP

后处理

  1. customThe resulting reaction mixture
  2. extractionThe aquoeus phase was extracted with ethyl acetate (3×100 mL)
  3. dry with materialThe combined organic layer dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated