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
- 0 °C
PROCEDURE
实验过程
To a mixture of 40.4 g (0.200 mole) of 3,5-dichloro-2,4,6-trifluoropyridine in 50 ml of dimethylformamide that had been cooled to 0° C. was added slowly 10 g (0.20 mole) of sodium cyanide. After addition was complete the reaction was stirred at 0° C. for two hours and at room temperature of two hours. The dimethylformamide was distilled from the reaction mixture under reduced pressure, and the black residue was mixed with 200 ml of water. This mixture was extracted with ethyl acetate. The extracts were combined, and the ethyl acetate was evaporated, leaving a black residue weighing approximately 15 g. This residue was distilled, yielding approximately 10 g of 4-cyano-3,5-dichloro-2,6-difluoropyridine as a white solid.
WORKUP
后处理
- additionAfter addition
- distillationThe dimethylformamide was distilled from the reaction mixture under reduced pressure
- additionthe black residue was mixed with 200 ml of water
- extractionThis mixture was extracted with ethyl acetate
- customthe ethyl acetate was evaporated
- customleaving a black residue
- distillationThis residue was distilled