HRID2080673

反应详情

EQUATION

反应方程式

HRID 2080673 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

43.3 g of 2-fluoro-4-nitrobenzoic acid was dissolved in 600 ml of dimethylformamide, and 1,1′-carbodiimide was added to it, and stirred at room temperature for 2 hours. 11.1 g of sodium borohydride was added thereto, and further stirred for 30 minutes. Aqueous saturated ammonium chloride solution was added to it, 800 ml of water was added thereto, extracted with 1.2 liters of ethyl acetate, and the organic layer was washed with saturated saline water. The solvent was evaporated away under reduced pressure, the residue was again diluted with ethyl acetate, and the organic layer was washed with water and saturated saline water. This was dried with anhydrous sodium sulfate, and the solvent was evaporated away to obtain 32.7 g of a brown oil.

WORKUP

后处理

  1. stirringfurther stirred for 30 minutes
  2. additionwas added
  3. extractionextracted with 1.2 liters of ethyl acetate
  4. washthe organic layer was washed with saturated saline water
  5. customThe solvent was evaporated away under reduced pressure
  6. additionthe residue was again diluted with ethyl acetate
  7. washthe organic layer was washed with water and saturated saline water
  8. dry with materialThis was dried with anhydrous sodium sulfate
  9. customthe solvent was evaporated away