HRID1500861

反应详情

EQUATION

反应方程式

HRID 1500861 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-(methylthio)-1H-pyrazolo[3,4-c]pyridine (10 g, 60.6 mmol) in DMF (100 mL) was added oxone (37 g, 121.2 mmol.) in portions. The reaction mixture was stirred at RT. After the reaction completed, water (100 mL) was added. The reaction was quenched carefully by addition of Na2SO3 and Na2CO3. The solid was filtered off and washed with MeOH (300 mL). The filtrate was concentrated under vacuum and the residue was purified by chromatography on silica gel column (DCM/MeOH=20/1) to give 3-(methylsulfonyl)-1H-pyrazolo[3,4-c]pyridine (10.7 g, yield: 90%) as a yellow solid. MS obsd. (ESI+) [(M+H)+] 198.0.

WORKUP

后处理

  1. customThe reaction was quenched carefully by addition of Na2SO3 and Na2CO3
  2. filtrationThe solid was filtered off
  3. washwashed with MeOH (300 mL)
  4. concentrationThe filtrate was concentrated under vacuum
  5. customthe residue was purified by chromatography on silica gel column (DCM/MeOH=20/1)