HRID1280554

反应详情

EQUATION

反应方程式

HRID 1280554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-(2,6-dichlorophenyl)-7-methylthio-1-methyl-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one (1.1) (5 g, 14.1 mmol) in 200 mL of dichloromethane was cooled in ice and treated with 3-chloroperbenzoic acid (10 g, 28.9 mmol). The mixture was stirred at room temperature for 17 hours, then treated with 2 mL of dimethyl sulfoxide and left to stand for 10 minutes. Saturated aqueous sodium bicarbonate solution (100 mL) was then added and the phases were separated. The organic phase was dried over magnesium sulfate and filtered. Concentration of the filtrate under reduced pressure gave 5 g (92%) of 3-(2,6-dichlorophenyl)-7-methanesulfonyl-1-methyl-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one (sulfone 1.2) as a white solid.

WORKUP

后处理

  1. waitleft
  2. waitto stand for 10 minutes
  3. customthe phases were separated
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. filtrationfiltered