HRID44242

反应详情

EQUATION

反应方程式

HRID 44242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 5-bromo-2-chloro-3-nitropyridine (5.0 g, 21.1 mmol) in methanol (50 mL) and dichloromethane (5 mL) was added zinc (7.6 g, 115.8 mmol) and ammonium chloride (5.6 g, 105.3 mmol). The reaction mixture was stirred for 24 hours. The solids were removed by filtration and washed with dichloromethane. The filtrate was washed with water (50 mL), brine (50 mL), dried over sodium sulfate, filtered and concentrated to dryness under reduced pressure. The crude 5-bromo-2-chloropyridin-3-amine (4.2 g) was used without further purification. LCMS [M+H]: 207.

WORKUP

后处理

  1. customThe solids were removed by filtration
  2. washwashed with dichloromethane
  3. washThe filtrate was washed with water (50 mL), brine (50 mL)
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure
  7. customThe crude 5-bromo-2-chloropyridin-3-amine (4.2 g) was used without further purification