HRID976228

反应详情

EQUATION

反应方程式

HRID 976228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

220.93 g of isopropyl mercaptan are added dropwise at a temperature of from 0° to -5° C. to a mixture of 388.6 g of potassium carbonate and 301 g of 2,3-difluoropyridine in 4300 ml of dimethylformamide. After stirring for 20 minutes, the temperature of the reaction mixture is allowed to rise slowly to room temperature and is stirred for a further 30 minutes. The reaction mixture is then added to an ice-water/ethyl acetate mixture, the phases are washed four times with ethyl acetate and ice-water and then dried over sodium sulfate. After filtering and concentrating by evaporation, the resulting crude product (510 g) is purified by column chromatography (ethyl acetated hexane 1:9) to give 327.3 g of 3-fluoro-2-isopropylthiopyridine in the form of an oil.

WORKUP

后处理

  1. customto rise slowly to room temperature
  2. stirringis stirred for a further 30 minutes
  3. washthe phases are washed four times with ethyl acetate and ice-water
  4. dry with materialdried over sodium sulfate
  5. filtrationAfter filtering
  6. concentrationconcentrating by evaporation
  7. customthe resulting crude product (510 g) is purified by column chromatography (ethyl acetated hexane 1:9)