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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
5-Chloro-4-(3′-cyano-3-(3-nitro-1H-pyrazol-4-yl)biphenyl-4-yloxy)-2-fluoro-N-(1,3,4-thiadiazol-2-yl)benzenesulfonamide (Preparation 62, 51 mg, 0.0853 mmol) was dissolved in acetonitrile (1 mL) and heated at 50° C. Potassium carbonate (58.8 mg, 0.426 mmol) followed by sodium dithionite (59.4 mg, 0.341 mmol) and water (1 mL) were added. The reaction mixture was heated at 50° C. for 2 hours, cooled to room temperature and partitioned between EtOAc (10 mL) and water (5 mL). The aqueous phase was separated and extracted with EtOAc (2×3 mL) and the combined organic phases were washed with a saturated solution of brine (3 mL), dried over MgSO4 and concentrated in vacuo. The crude residue was purified by reverse phase HPLC.
WORKUP
后处理
- additionwere added
- temperatureThe reaction mixture was heated at 50° C. for 2 hours
- temperaturecooled to room temperature
- custompartitioned between EtOAc (10 mL) and water (5 mL)
- customThe aqueous phase was separated
- extractionextracted with EtOAc (2×3 mL)
- washthe combined organic phases were washed with a saturated solution of brine (3 mL)
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customThe crude residue was purified by reverse phase HPLC