HRID37882
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
22.0 g (144 mmol) of (6-chloropyridin-3-yl)acetonitrile are added to a mixture of 270 ml of ethanol and 101 ml conc. sulfuric acid, and the mixture is stirred under reflux for 24 h. With stirring, the reaction mixture is then slowly added dropwise to a mixture of 350 g of sodium bicarbonate and 1 liter of water. The aqueous phase is extracted with dichloromethane (five times 400 ml each). The combined organic phases are dried over sodium sulfate, filtered and freed from the solvent using a rotary evaporator. This gives 23.1 g (80% of theory) of the title compound, which is reacted without further purification.
WORKUP
后处理
- temperatureunder reflux for 24 h
- stirringWith stirring
- extractionThe aqueous phase is extracted with dichloromethane (five times 400 ml each)
- dry with materialThe combined organic phases are dried over sodium sulfate
- filtrationfiltered
- customa rotary evaporator
- customThis gives 23.1 g (80% of theory) of the title compound, which is reacted without further purification