HRID1024601

反应详情

EQUATION

反应方程式

HRID 1024601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 5-(4-chloro-phenyl)-6-(4-methylsulfanyl-phenyl)-1-phenyl-1,5-dihydro-pyrazolo[3,4-d]pyrimidin-4-one (2.10 g, 4.72 mmol) in dry dichloromethane (36 mL) and methanol (12 mL), magnesium monoperoxy phthalate hexahydrate (1.16 g, 2.36 mmol) is added at 0° C. and the resulting mixture is stirred for 3 h at that temperature. The reaction mixture is quenched with the addition of 10% sodium bicarbonate solution and extracted with dichloromethane (3×). The organic part separated is dried (Na2SO4) and concentrated. The crude product is purified by column chromatography (silica gel, 60-120 mesh) to afford 5-(4-chloro-phenyl)-6-(4-methanesulfinyl-phenyl)-1-phenyl-1,5-dihydro-pyrazolo[3,4-d]pyrimidin-4-one.

WORKUP

后处理

  1. customThe reaction mixture is quenched with the addition of 10% sodium bicarbonate solution
  2. extractionextracted with dichloromethane (3×)
  3. customThe organic part separated
  4. dry with materialis dried (Na2SO4)
  5. concentrationconcentrated
  6. customThe crude product is purified by column chromatography (silica gel, 60-120 mesh)