HRID654019

反应详情

EQUATION

反应方程式

HRID 654019 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

8.36 g (20 mmol) of 3-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]-benzenesulfonic acid chloride is dissolved in 40 ml of tetrahydrofuran, 2.52 g (25 mmol) of triethylamine and 4.03 (25 mmol) of 2-hydroxy-2-(2,2-dimethyl-1,3-dioxolan-4-yl)-N-methylethylamine are added and stirred for 3 hours at 45° C. The reaction mixture is then concentrated by evaporation under reduced pressure, the residue is extracted with ethyl acetate and the extract is chromatographed on silica gel 60 (Merck) with ethyl acetate/hexane. 9.35 g (16.8 mmol)=84% of the theoretical yield is obtained as an amorphous solid.

WORKUP

后处理

  1. concentrationThe reaction mixture is then concentrated by evaporation under reduced pressure
  2. extractionthe residue is extracted with ethyl acetate
  3. customthe extract is chromatographed on silica gel 60 (Merck) with ethyl acetate/hexane
  4. custom9.35 g (16.8 mmol)=84% of the theoretical yield
  5. customis obtained as an amorphous solid