反应详情

To a solution of 2,6-dibromopyridin-4-amine (1.0 g, 3.97 mmol), DMAP (0.048 g, 0.397 mmol), and pyridine (0.482 mL, 5.95 mmol) in THF (7.94 mL) at rt was slowly added acetic anhydride (0.412 mL, 4.37 mmol), and the mixture was stirred at rt for 16 h, after which time the reaction was heated to 65° C. for a period of 5 days. After cooling to rt, MeOH (5 mL) was added and the reaction was concentrated under reduced pressure. The product was purified by silica gel chromatography using a gradient solvent system of 0-100% EtOAc/Hexanes. The product-containing fractions were collected and concentrated under reduced pressure to give N-(2,6-dibromopyridin-4-yl)acetamide (1.10 g, 94%) as a yellow solid. MS ESI calcd for C7H6Br2N2O [M+H]+ 293, found 293.

1. customat rt
2. temperatureafter which time the reaction was heated to 65° C. for a period of 5 days
3. temperatureAfter cooling to rt
4. concentrationthe reaction was concentrated under reduced pressure
5. customThe product was purified by silica gel chromatography
6. customThe product-containing fractions were collected
7. concentrationconcentrated under reduced pressure