反应详情

A suspension of 5-bromo-2-chloro-3-nitropyridine (3.79 g, 16 mmol), 1-(3-aminophenyl)pyrrolidin-2-one (2.56 g, 15 mmol) and potassium carbonate (2.0 g, 15 mmol) in 1,2-dichloroethane (25 ml) was heated at reflux for 60 hours. The reaction was cooled, diluted with dichloromethane (200 ml) and extracted with water. The organic phase was then dried over anhydrous sodium sulphate, filtered and pre-adsorbed on to silica (25 g). Purification by column chromatography eluting with isohexane on a gradient of ethyl acetate (10%-40%) gave 1-[3-(5-bromo-3-nitropyridin-2-ylamino)phenyl]pyrrolidin-2-one as a red solid (3.7 g, 68%).

1. temperaturewas heated
2. temperatureat reflux for 60 hours
3. temperatureThe reaction was cooled
4. extractionextracted with water
5. dry with materialThe organic phase was then dried over anhydrous sodium sulphate
6. filtrationfiltered and pre-adsorbed on to silica (25 g)
7. customPurification by column chromatography
8. washeluting with isohexane on a gradient of ethyl acetate (10%-40%)