反应详情

To a solution of (4-(5-(4-chlorophenyl)-4-oxo-1-phenyl-4,5-dihydro-1H-pyrazolo[3,4-d]pyrimidin-6-yl)phenylthio)methyl acetate (1.00 g, 1.98 mmol) in dry dichloromethane (30 mL) and methanol (10 mL), magnesium monoperoxy phthalate hexahydrate (1.08 g, 2.18 mmol) is added at 0° C. and the resulting mixture is stirred for 18 h at rt. Then 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 (4-(5-(4-chlorophenyl)-4-oxo-1-phenyl-4,5-dihydro-1H-pyrazolo[3,4-d]pyrimidin-6-yl)phenylsulfonyl)methyl acetate.

1. customThen the 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)