HRID2110987
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
Aluminium chloride (2 g) was suspended in 3 ml of fluorobenzene. A solution of 6-chloronicotinoyl chloride (1 g, 5.7 mmol) in 2 ml of fluorobenzene was added to the stirred reaction mixture by syringe and stirred at 80° C. overnight in a closed vial. The reaction mixture was deluted with EtOAc and basified with aqueous sodium hydroxide (pH>8.5). The precipitate formed was removed by filtration. The organic solution was washed with water, dried over magnesium sulfate and concentrated by rotary evaporation. Desired product was purified by column chromatography on silica (EtOAc/hexane) to give 1.22 g (90%).
WORKUP
后处理
- customThe precipitate formed
- customwas removed by filtration
- washThe organic solution was washed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated by rotary evaporation
- customDesired product was purified by column chromatography on silica (EtOAc/hexane)
- customto give 1.22 g (90%)