HRID44242
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
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
- customThe solids were removed by filtration
- washwashed with dichloromethane
- washThe filtrate was washed with water (50 mL), brine (50 mL)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated to dryness under reduced pressure
- customThe crude 5-bromo-2-chloropyridin-3-amine (4.2 g) was used without further purification