反应详情

温度

80 °C

A mixture of 3-chloro-2-hydroxy-5-nitropyridine (36.0 g), acetonitrile (72 mL), and phosphorus oxychloride (37.5 g) was heated to 80° C. The reaction was then stirred at this temperature for about 15 hours. After cooling the reaction to 40° C., water (27 g) was added, while maintaining the temperature below 70° C. The temperature was adjusted to 45° C., and then more water (189 g) was added slowly. The reaction was then cooled to 23° C., stirred for at least 12 hours, and then filtered. After washing the wet cake with water, the product was dried in a vacuum oven. 1H NMR (400 MHz/CDCl3) δ 9.10 (d, J=2.5 Hz, 1H), 8.56 (d, J=2.4 Hz, 1H)

1. temperatureAfter cooling
2. customthe reaction to 40° C.
3. temperaturewhile maintaining the temperature below 70° C
4. customwas adjusted to 45° C.
5. temperatureThe reaction was then cooled to 23° C.
6. stirringstirred for at least 12 hours
7. filtrationfiltered
8. washAfter washing the wet cake with water
9. customthe product was dried in a vacuum oven