HRID1719786

反应详情

EQUATION

反应方程式

HRID 1719786 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 20.6 g (0.1 mol) of 3-chloroperoxybenzoic acid in 100 ml of methylene chloride is cooled to a temperature of between -15° C. and -20° C., and there is then added dropwise a solution of 20.6 g (0.1 mol) of 2-methylthio-4-difluoromethoxy-6-methylpyrimidine in 50 ml of methylene chloride. After the reaction mixture has been stirred for 1 hour at the same temperature, it is diluted with methylene chloride; it is subsequently washed with a sodium hydrogen carbonate solution and water, dried over sodium sulfate and concentrated by evaporation. Crystallisation of the residue from a methylene chloride/petroleum ether mixture yields 21.6 g (97% of theory) of 2-methylsulfinyl-4-difluoromethoxy-6-methylpyrimidine, m.p. 105°-107° C.

WORKUP

后处理

  1. temperatureis cooled to a temperature of between -15° C. and -20° C., and there
  2. washit is subsequently washed with a sodium hydrogen carbonate solution and water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated by evaporation
  5. customCrystallisation of the residue from a methylene chloride/petroleum ether mixture