HRID1809692

反应详情

EQUATION

反应方程式

HRID 1809692 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

m-CPBA (797 mg, 4.62 mmol) was added slowly to a solution of 2-[3-(2-Methylsulfanyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-ylamino]-ethanol (from Example 20 supra) (0.7 g, crude) in a mixture of dichloromethane and methanol (40 mL, 1:1). The reaction mixture was stirred at room temperature for 30 minutes. The solvent was then removed under reduced pressure and the solid was purified by column chromatography (silica gel, 10 g, 200-300 mesh, eluting with dichloromethane:methanol, 5:1) to afford 2-[3-(2-methanesulfinyl-pyrimidin-4-yl)-1H-pyrazolo[3,4-d]pyrimidin-6-ylamino]-ethanol (Yield 1.9 g, crude). LC-MS: [M+H]+ 320.

WORKUP

后处理

  1. customThe solvent was then removed under reduced pressure
  2. customthe solid was purified by column chromatography (silica gel, 10 g, 200-300 mesh, eluting with dichloromethane:methanol, 5:1)