HRID1741003

反应详情

EQUATION

反应方程式

HRID 1741003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturecooled
  2. extractionThe mixture was extracted twice with 250 ml of diethyl ether
  3. washThe extracts were washed with water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated