HRID1719784

反应详情

EQUATION

反应方程式

HRID 1719784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution of 70.0 g (0.44 mol) of potassium permanganate in 700 ml of water is added dropwise to a solution of 30.9 g (0.15 mol) of 2-methylthio-4-difluoromethoxy-6-methylpyrimidine, 0.75 g of 18-crown-6-ether and 30 ml of glacial acetic acid in 1400 ml of methylene chloride. This mixture is stirred for 3 hours at a temperature of between 20° and 25° C., and sodium hydrogen sulfite solution is then added until the precipitated manganese oxide (MnO2) is dissolved. The organic phase of the reaction mixture is separated, washed with water, dried over sodium sulfate and concentrated by evaporation. There are thus obtained, as a colourless residue, 33.8 g (95% of theory) of 2-methylsulfonyl-4-difluoromethoxy-6-methylpyrimidine, m.p. 86°-88° C.

WORKUP

后处理

  1. dissolutionis dissolved
  2. customThe organic phase of the reaction mixture is separated
  3. washwashed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated by evaporation