反应详情

A mixture of 0.50 g of 5-iodo-N2-methylpyridine-2,3-diamine and 6 ml of trifluoroacetic acid was stirred at room temperature for 1 hour, and then stirred under heat-reflux for 9 hours. The cooled reaction mixture was concentrated under reduced pressure, then water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with water, then dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 0.57 g of 6-iodo-3-methyl-2-trifluoromethyl-3H-imidazo[4,5-b]pyridine.

1. stirringstirred
2. temperatureunder heat-reflux for 9 hours
3. customThe cooled reaction mixture
4. concentrationwas concentrated under reduced pressure
5. additionwater was added
6. extractionthe mixture was extracted with ethyl acetate
7. washThe organic layer was washed with water
8. dry with materialdried over anhydrous sodium sulfate
9. concentrationconcentrated under reduced pressure