HRID1534174

反应详情

EQUATION

反应方程式

HRID 1534174 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

25 ml of trifluoroacetic acid are added at a temperature of 0° C. to a solution of 3.88 g of 2-(2-fluoroethylthio)-N-tert.-butylphenylsulfonamide, obtained in accordance with Example P1, in 25 ml of trichloromethane. After stirring for 18 hours at a temperature of +25° C., the resulting brown reaction mixture is lyophilised. After chromatographic purification of the oily residue with 1) ethyl acetate/petroleum ether (1:1) over silica gel and 2) dichloromethane/acetone (9:1) over silica gel, the resulting fractions are concentrated by evaporation to give 1.5 g (60.5% of the theoretical yield) of crystalline 2-(2-fluoroethylthio)-phenylsulfonamide.

WORKUP

后处理

  1. customAfter chromatographic purification of the oily residue with 1) ethyl acetate/petroleum ether (1:1) over silica gel and 2) dichloromethane/acetone (9:1) over silica gel
  2. concentrationthe resulting fractions are concentrated by evaporation
  3. customto give 1.5 g (60.5% of the