HRID636067

反应详情

EQUATION

反应方程式

HRID 636067 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

20 g (0.0693 mol) of 95% pure 3-fluoro-2-phenylthio-5-trifluoromethylpyridine were introduced into 100 ml of glacial acetic acid and 20 ml of trifluoroacetic acid and over a period of 5 min, with stirring at 22° C., 5.64 g (0.083 mol) of 50% strength hydrogen peroxide were added. The reaction mixture was stirred at 22° C. for 10 h and then poured into 1 l of ice-water and extracted with methylene chloride. The organic phase was washed with saturated sodium bicarbonate solution and water. After drying, filtration through silica gel and concentration under reduced pressure, 19.1 g (95.4% of theory) of the title compound of 24 n D

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at 22° C. for 10 h
  2. extractionextracted with methylene chloride
  3. washThe organic phase was washed with saturated sodium bicarbonate solution and water
  4. customAfter drying
  5. filtrationfiltration
  6. concentrationthrough silica gel and concentration under reduced pressure, 19.1 g (95.4% of theory) of the title compound of 24 n D