HRID1672645
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureheated
- temperatureunder reflux for 12 hours
- temperatureThe mixture is then cooled
- filtrationfiltered
- washwashed with dichloromethane
- concentrationconcentrated
- customthe residue is purified by chromatography (silica gel; mobile phase: cyclohexane/ethyl acetate 5:1)