反应详情

A mixture of 10.0 g of N2-methyl-5-trifluoromethylsulfanylpyridine-2,3-diamine, 41 ml of formic acid and 5 ml of water was stirred under heating and refluxing for 2 hours. The reaction mixture was concentrated under reduced pressure, a saturated aqueous sodium bicarbonate solution was added to the resulting residue, and the mixture was extracted with methyl-tert-butyl ether. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was applied to a silica gel column chromatography to obtain 7.80 g of 3-methyl-6-trifluoromethylsulfanyl-3H-imidazo[4,5-b]pyridine.

1. temperatureunder heating
2. temperaturerefluxing for 2 hours
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additiona saturated aqueous sodium bicarbonate solution was added to the resulting residue
5. extractionthe mixture was extracted with methyl-tert-butyl ether
6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure