HRID1500861
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe reaction was quenched carefully by addition of Na2SO3 and Na2CO3
- filtrationThe solid was filtered off
- washwashed with MeOH (300 mL)
- concentrationThe filtrate was concentrated under vacuum
- customthe residue was purified by chromatography on silica gel column (DCM/MeOH=20/1)