HRID1090116

反应详情

EQUATION

反应方程式

HRID 1090116 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(4-fluorophenyl)-4-methyl-5-hydroxymethyl-1,2,3-triazole (871 mg; 4.20 mmol), prepared as described in example 6, and thionyl chloride (400 ml; 5.46 mmol) in benzene (14 ml) was heated under reflux for 4 hours. The reaction mixture was kept under stirring at room temperature overnight, thionyl chloride and benzene were evaporated and the resultant crude compound was collected several times with benzene. After evaporation of the solvent, the crude compound was purified by chromatography on silica gel (230-400 mesh), eluent methylene chloride:acetone=95:5, giving the title compound (m.p. 70°-71° C.).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. customthionyl chloride and benzene were evaporated
  4. customthe resultant crude compound was collected several times with benzene
  5. customAfter evaporation of the solvent
  6. customthe crude compound was purified by chromatography on silica gel (230-400 mesh), eluent methylene chloride