HRID705840
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
- 70 °C
PROCEDURE
实验过程
To a solution of 3-(4-(4-fluorophenoxyl)phenyl)acrylonitrile (5 g, 20.90 mmol) in ethanol (80 mL) was added NaBH4 (5.44 g, 144 mmol). The mixture was heated at 70° C. overnight. After cooling to room temperature, the reaction mixture was quenched with water (50 mL), and ethanol was removed under reduced pressure. The residue was partitioned between EA (100 mL) and water (50 mL). The organic phase was washed with saturated NaHCO3 solution (80 mL), brine (50 mL), dried over sodium sulfate, concentrated, and purified via flash chromatography to afford the title compound (4.7 g, 16.48 mmol, 79% yield) as a white solid. LCMS: rt=1.55 min, [M+H+]=242
WORKUP
后处理
- temperatureAfter cooling to room temperature
- customthe reaction mixture was quenched with water (50 mL), and ethanol
- customwas removed under reduced pressure
- customThe residue was partitioned between EA (100 mL) and water (50 mL)
- washThe organic phase was washed with saturated NaHCO3 solution (80 mL), brine (50 mL)
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- custompurified via flash chromatography