反应详情

温度

52.5 °C

A 5 L flask with mechanical stirrer, thermocouple, and addition funnel was charged with 2-hydroxy-5-nitropyridine (200 g) and concentrated HCl (890 mL). The mixture was warmed to 50-55° C. and a solution of KClO3 (61.3 g, 0.5 mol) in water (850 mL) was added dropwise over 75 minutes maintaining the reaction temperature at 55-59° C. Following complete addition, the reaction mixture was cooled in an ice-water bath to an internal temperature of <6° C. and then filtered. The filter cake was washed with cold water (700 mL) and dried under vacuum at 50° C. for 12 hours to provide the title compound. 1H NMR (CDCl3, 300 MHz) δ 7.43 (d, J=3 Hz, 1H), 7.59 (d, J=3 Hz, 1H).

1. additionA 5 L flask with mechanical stirrer, thermocouple, and addition funnel
2. temperaturemaintaining the reaction temperature at 55-59° C
3. additionaddition
4. temperaturethe reaction mixture was cooled in an ice-water bath to an internal temperature of <6° C.
5. filtrationfiltered
6. washThe filter cake was washed with cold water (700 mL)
7. customdried under vacuum at 50° C. for 12 hours