HRID2166102

反应详情

EQUATION

反应方程式

HRID 2166102 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

9.3 g of 4-phenoxyphenol and 9 g of potassium carbonate are stirred in 75 ml of anhydrous dimethylformamide for 1 hour at 80° C. Subsequently, 6.6 g of 2-chloromethyl-5-methyl-1,3,4-oxadiazole in 20 ml of anhydrous dimethylformamide is dripped in. The mixture is stirred for 10 hours at 80° C. and at room temperature (approx. 20° C.) overnight. The mixture is then stirred into 500 ml of ice water and extracted three times with ethyl acetate. After drying over sodium sulfate and removal of the solvent, the residue is purified by chromatography over silica gel using n-hexane/ethyl acetate (4:1) as eluant. There is obtained 12 g of 5-methyl-2-[(4-phenoxyphenoxy)-methyl]-1,3,4-oxadiazole; colorless crystals; m.p.: 78°-79° C.

WORKUP

后处理

  1. extractionextracted three times with ethyl acetate
  2. dry with materialAfter drying over sodium sulfate and removal of the solvent
  3. customthe residue is purified by chromatography over silica gel