反应详情

温度

50 °C

To a 250 mL flask were added 6-hydroxynicotinic acid (20 g, Aldrich) and 100 mL of red fuming nitric acid. The mixture was slowly heated to 50° C. (bath temperature) and stirred at this temperature for 8 h. Then the temperature was slowly raised to 80° C. and the mixture was stirred for another 7 h. The mixture was cooled to rt overnight and the yellow precipitate was collected by filtration, washed with water (10 mL) and dried. LC-MS: >95% pure. 1H NMR (CD3OD, 400 MHz): δ=8.45 (d, J=2.5 Hz, 1H), 8.85 (d, J=2.5 Hz, 1H).

1. temperatureThen the temperature was slowly raised to 80° C.
2. stirringthe mixture was stirred for another 7 h
3. temperatureThe mixture was cooled to rt overnight
4. filtrationthe yellow precipitate was collected by filtration
5. washwashed with water (10 mL)
6. customdried