反应详情

温度

75 °C

A sealed tube was charged with 4-aminonicotinic acid 45 (8.00 g, 57.9 mmol), acetic acid (75 mL) and water (75 mL). The reaction was heated at 75° C. and stirred vigorously until homogeneous. After cooling to 50° C., bromine (10.0 mL, 195 mmol) was added and stirring continued for 16 h. Upon cooling to 0° C., the resulting orange precipitate was collected by filtration, rinsed with H2O, and dried under vacuum to give 46 (10.5 g, 84% yield).

1. temperatureAfter cooling to 50° C.
2. stirringstirring
3. temperatureUpon cooling to 0° C.
4. filtrationthe resulting orange precipitate was collected by filtration
5. washrinsed with H2O
6. customdried under vacuum