反应详情

温度

100 °C

Nitric acid (9 ml) was slowly added dropwise to a suspension of 3-methylxanthine (10 g) in acetic acid (180 ml) at 100° C., and the resulting white suspension was stirred at 100° C. for 30 minutes followed by 140° C. for 20 minutes. After cooling the reaction solution to room temperature, the solvent was removed by distillation at reduced pressure at 60° C. to give a yellow solid. The resulting yellow solid was washed with water, and recrystallization from 0.5 M hydrochloric acid gave a pale yellow solid. A suspension of the solid in concentrated hydrochloric acid (500 ml) was stirred at 110° C. for 15 minutes, then the reaction solution was cooled to room temperature, and the solvent was removed by distillation at reduced pressure to give a yellow-white solid. Recrystallization of the resulting solid from water gave 6.75 g of the title compound.

1. waitfollowed by 140° C. for 20 minutes
2. temperatureAfter cooling the reaction solution to room temperature
3. customthe solvent was removed by distillation at reduced pressure at 60° C.
4. customto give a yellow solid
5. washThe resulting yellow solid was washed with water, and recrystallization from 0.5 M hydrochloric acid
6. customgave a pale yellow solid
7. stirringwas stirred at 110° C. for 15 minutes
8. temperaturethe reaction solution was cooled to room temperature
9. customthe solvent was removed by distillation at reduced pressure
10. customto give a yellow-white solid
11. customRecrystallization of the resulting solid from water