HRID1073954

反应详情

EQUATION

反应方程式

HRID 1073954 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

3.77 g of m-chloroperbenzoic acid were added to a solution of 4.78 g of 4-[2-hydroxy-1,1-dimethyl-3-(4pyrimidinyl)propoxy]benzonitrile in 75 ml of dichloromethane and the mixture was stirred at 20° C. for 16 hours. A further 0.38 g of m-chloroperbenzoic acid was added and the mixture was stirred at 20° C. for 24 hours. The mixture was then washed in succession with water and sodium chloride solution. The organic solution was evaporated and the residue was chromatographed on silica gel using diethyl ether/methanol (9:1) for the elution to give 0.98 g of 6-[3-(4-cyanophenoxy)-2-hydroxy-3-methylbutyl]pyrimidine 1-oxide in the form of a white solid of melting point 105°-107.5° C. (from ethyl acetate).

WORKUP

后处理

  1. stirringthe mixture was stirred at 20° C. for 24 hours
  2. washThe mixture was then washed in succession with water and sodium chloride solution
  3. customThe organic solution was evaporated
  4. customthe residue was chromatographed on silica gel
  5. washfor the elution