反应详情

温度

53 °C

Concentrated hydrochloric acid (239 g) was added to 2-hydroxy-5-nitropyridine (40.0 g). The resulting slurry was heated to 53° C., and stirred until all the solids dissolved. To this was slowly added a solution of potassium chlorate (14.0 g) in water (250 g), while maintaining the temperature between 55° C. and 59° C. The resulting mixture was stirred at 58-62° C. for about 1 hour. The reaction was then cooled to room temperature, stirred for 12 hours and then filtered. After washing the wet cake with water, the product was dried in a vacuum oven. 1H NMR (400 MHz/DMSO-d6) δ 8.64 (d, J=2.9 Hz, 1H), 8.35 (d, J=2.9 Hz, 1H)

1. dissolutiondissolved
2. temperaturewhile maintaining the temperature between 55° C. and 59° C
3. stirringThe resulting mixture was stirred at 58-62° C. for about 1 hour
4. temperatureThe reaction was then cooled to room temperature
5. stirringstirred for 12 hours
6. filtrationfiltered
7. washAfter washing the wet cake with water
8. customthe product was dried in a vacuum oven