HRID2110987

反应详情

EQUATION

反应方程式

HRID 2110987 的结构方程式

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

  1. customThe precipitate formed
  2. customwas removed by filtration
  3. washThe organic solution was washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated by rotary evaporation
  6. customDesired product was purified by column chromatography on silica (EtOAc/hexane)
  7. customto give 1.22 g (90%)