HRID1672645

反应详情

EQUATION

反应方程式

HRID 1672645 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7.50 g (44.08 mmol) of methyl 5-fluoro-2-hydroxybenzoate in 40 ml of dry acetonitrile is mixed with 9.44 g (48.49 mmol) of 2-trifluoromethylbenzyl chloride and 18.28 g (132.25 mmol) of anhydrous potassium carbonate and heated under reflux for 12 hours. The mixture is then cooled, filtered, washed with dichloromethane and concentrated, and the residue is purified by chromatography (silica gel; mobile phase: cyclohexane/ethyl acetate 5:1). 9.18 g (28 mmol, 89% purity, 56% yield) of the title compound are obtained.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux for 12 hours
  3. temperatureThe mixture is then cooled
  4. filtrationfiltered
  5. washwashed with dichloromethane
  6. concentrationconcentrated
  7. customthe residue is purified by chromatography (silica gel; mobile phase: cyclohexane/ethyl acetate 5:1)