HRID2209030
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-chloro-3-(difluoromethyl)-4-(methylthio)-3H-imidazo[4,5-c]pyridine (431 mg, 1.73 mmol) in DCM (12 mL) was added m-CPBA (max. 77%, 1.1 g, 4.9 mmol). After stifling 4 h, saturated aqueous sodium thiosulfate (30 mL) was added and the biphasic mixture was stirred 15 min. The mixture was diluted with EtOAc (30 mL) and water (30 mL). The phases were separated, and the organic layer was washed with saturated NaHCO3 (2×50 mL), dried over Na2SO4, filtered, and concentrated to afford 6-chloro-3-(difluoromethyl)-4-(methylsulfonyl)-3H-imidazo[4,5-c]pyridine 2.63 that was used without further purification. LCMS-ESI+ (m/z): [M+H]+ calcd for C8H7ClF2N3O2S: 282.0; found: 282.0.
WORKUP
后处理
- customThe phases were separated
- washthe organic layer was washed with saturated NaHCO3 (2×50 mL)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated