HRID1858183

反应详情

EQUATION

反应方程式

HRID 1858183 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5 g (14.1 mmol) of 3-(2,6-dichlorophenyl)-7-methylthio-3,4-dihydro-1-methylpyrimido[4,5-d]pyrimidin-2(1H)-one in 200 ml of dichloromethane was cooled in ice and treated with 10 g (28.9 mmol) of 3-chloroperbenzoic acid. 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. 100 ml of saturated aqueous sodium bicarbonate solution were 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-3,4-dihydro-1-methylpyrimido[4,5-d]pyrimidin-2(1H)-one 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