HRID1097245
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
- 55 °C
PROCEDURE
实验过程
To a solution of 6-bromo-3-fluoro-2-methylpyridine (0.5 gr, 2.63 mmol) in dichloromethane (5 ml) were added at room temperature N-bromosuccinimide (937 mg, 5.26 mmol) and azo-di-isobutyronitrile (86 mg, 0.526 mmol). After 17 h stirring at 55° C. the reaction mixture was quenched by the addition of water and the product was extracted into dichloromethane. The combined organic phases were washed with brine, dried over sodium sulfate and concentrated under reduced pressure. Column chromatography afforded 6-bromo-2-(bromomethyl)-3-fluoropyridine (388 mg) as a clear oil.
WORKUP
后处理
- customwas quenched by the addition of water
- extractionthe product was extracted into dichloromethane
- washThe combined organic phases were washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure