HRID474598

反应详情

EQUATION

反应方程式

HRID 474598 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a solution of 3-(4-(4-fluorophenoxy)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

  1. temperatureAfter cooling to room temperature
  2. customthe reaction mixture was quenched with water (50 mL), and ethanol
  3. customwas removed under reduced pressure
  4. customThe residue was partitioned between EA (100 mL) and water (50 mL)
  5. washThe organic phase was washed with saturated NaHCO3 solution (80 mL), brine (50 mL)
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated
  8. custompurified via flash chromatography