反应详情

温度

15 °C

Propionitrile (656 ml), 2,3-dichloro-5-trifluoromethylpyridine (87.5 g) and 4-dimethylaminopyridine (52 g) were heated at reflux for 5 hours under nitrogen. The mixture was cooled and a solution of sodium cyanide (30 g) in water (110 ml) added at 15° C. After stirring at 15° C. for 5 hours the reaction was complete and water (250 ml) added to dissolve the inorganic salts. The organic phase was washed with water followed by extraction with 2N HCl to remove 4-dimethylaminopyridine. Propionitrile was removed by vacuum distillation at 40° C. to give the product, 3-chloro-2-cyano-5-trifluoromethylpyridine in 73 to 84% yield.

1. temperatureat reflux for 5 hours under nitrogen
2. temperatureThe mixture was cooled
3. dissolutionto dissolve the inorganic salts
4. washThe organic phase was washed with water
5. extractionfollowed by extraction with 2N HCl
6. customto remove 4-dimethylaminopyridine
7. customPropionitrile was removed by vacuum distillation at 40° C.