HRID1019733

反应详情

EQUATION

反应方程式

HRID 1019733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-(2-Chloro 4-nitro-phenyl)acetaldehyde (3.0 g, 15.03 mmol) and 4-fluorobenzylamine (1.88 g, 15.02 mmol) were added to methanol (45 mL) at RT and stirred for 15 minutes. The reaction mixture was cooled to 0° C. and acetic acid (15 mL) followed by solid NaBH4 (0.56 g, 15.0 mmol) were added. The reaction mixture was allowed to warm to RT and stirring continued for 2 hours. The volatiles were then removed under reduced pressure. Dichloromethane (60 mL) and water (60 mL) were added and the mixture was stirred for 15 minutes. The separated organic layer was washed with water (60 mL), brine (60 mL), dried (Na2SO4) and the solvents removed under reduced pressure to afford the title compound (3.1 g, 67%) which was used in the next step without further purification.

WORKUP

后处理

  1. additionwere added
  2. temperatureto warm to RT
  3. stirringstirring
  4. waitcontinued for 2 hours
  5. customThe volatiles were then removed under reduced pressure
  6. additionDichloromethane (60 mL) and water (60 mL) were added
  7. stirringthe mixture was stirred for 15 minutes
  8. washThe separated organic layer was washed with water (60 mL), brine (60 mL)
  9. dry with materialdried (Na2SO4)
  10. customthe solvents removed under reduced pressure