反应详情

Chloroacetyl chloride (95.5 ml) is dissolved in dichloromethane (500 ml), and thereto is added dropwise a suspension of 2-amino-5-chloropyridine (128.6 g) and triethylamine (169 ml) in dichloromethane (1000 ml) under ice-cooling. The reaction solution is warmed to room temperature and stirred for 0.5 hours. The reaction solution is concentrated under reduced pressure, and thereto is poured ice-water, followed by extraction with ethyl acetate. The organic layer is washed with saturated brine, dried over sodium sulfate and treated with activated charcoal. After filtration to remove insoluble materials, the filtrate is concentrated under reduced pressure and the resulting residue is suspended in diisopropyl ether. The precipitates are collected by filtration, washed with diisopropyl ether and dried to give the title compound (153.4 g).

1. additionis added dropwise
2. temperaturecooling
3. concentrationThe reaction solution is concentrated under reduced pressure
4. additionis poured ice-water
5. extractionfollowed by extraction with ethyl acetate
6. washThe organic layer is washed with saturated brine
7. dry with materialdried over sodium sulfate
8. additiontreated with activated charcoal
9. filtrationAfter filtration
10. customto remove insoluble materials
11. concentrationthe filtrate is concentrated under reduced pressure
12. filtrationThe precipitates are collected by filtration
13. washwashed with diisopropyl ether
14. customdried