HRID1741003
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
p-Fluorophenol (1.66 g, 14.81 mmol) and ethyl p-fluorobenzoate (2.50 g, 14.87 mmol) were dissolved in 30 ml of dry DMSO and treated with 1.7 g of KF/alumina and 0.39 g of crown ether (18-C-6). The reaction mixture was heated at 100° C. for sixty hours, cooled and poured into 100 ml of water. The mixture was extracted twice with 250 ml of diethyl ether. The extracts were washed with water and then brine, combined, dried over MgSO4 and concentrated. Medium-pressure liquid chromatography over silica using 30:1 hexane/ethyl acetate afforded 2.32 g (60% yield) of the subtitle compound.
WORKUP
后处理
- temperaturecooled
- extractionThe mixture was extracted twice with 250 ml of diethyl ether
- washThe extracts were washed with water
- dry with materialdried over MgSO4
- concentrationconcentrated