HRID879296
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 6-bromo-1H-pyrazolo[4,3-b]pyridine (200 mg, 1.01 mmol) in DMF (5 mL) was added cesium carbonate (494 mg, 1.515 mmol). The reaction solution was stirred at room temperature for 5 minutes, iodomethane (215 mg, 1.515 mmol) was added. The reaction solution was stirred for 2 h and quenched with water. Volatiles were removed and the residue partitioned between ethyl acetate and water. The organic phase was washed with brine, dried (MgSO4), filtered and concentrated to give crude product which was purified by chromatographic column to afford the desired product 6-bromo-1-methyl-1H-pyrazolo[4,3-b]pyridine. LCMS-ESI+: calc'd for C7H6BrN3: 211.98 (M+H+); Found: 212.1 (M+H+).
WORKUP
后处理
- stirringThe reaction solution was stirred for 2 h
- customquenched with water
- customVolatiles were removed
- customthe residue partitioned between ethyl acetate and water
- washThe organic phase was washed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customto give crude product which
- customwas purified by chromatographic column