HRID735060

反应详情

EQUATION

反应方程式

HRID 735060 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.7 mL (40.32 mmol) of trifluoromethanesulfonic acid anhydride dissolved in 5 mL dichloromethane is added dropwise between −10° C. to −5° C. to a solution of 7.5 g (36.65 mmol) of 3-chlorobiphenyl-4-ol and 6.1 mL (44 mmol) of triethylamine in 100 mL of dichloromethane. Then the mixture is stirred for 30 minutes. The reaction solution is then extracted with water, the organic phase is separated off and filtered through an Alox frit. The filtrate is concentrated by evaporation. Yield: 12 g (97% of theory); C13H8ClF3O3S (M=336.72); calc.: molecular ion peak (M+H)+: 336/338 (Cl); found: molecular ion peak (M+H)+: 336/338 (Cl); Rf value: 0.7 (silica gel, petroleum ether/ethyl acetate (5:1)).

WORKUP

后处理

  1. extractionThe reaction solution is then extracted with water
  2. customthe organic phase is separated off
  3. filtrationfiltered through an Alox frit
  4. concentrationThe filtrate is concentrated by evaporation