反应详情

温度

0 °C

The title compound was prepared using an adaptation of the method of Cheeseman (Cheeseman, G. W. H., J. Chem. Soc. 1171 (1962)). 6-Fluoro-1,4-dihydroquinoxaline-2,3-dione (200 mg, 1.10 mmol) was dissolved in 3 mL of concentrated H2SO4 and the blue green solution was cooled to 0° C. with stirring. To this was added in small portions KNO3 (110 mg, 1.10 mmol). The reaction was allowed to stir 1 h at 0° C. and then was allowed to come to room temperature and stir overnight. The brown-orange reaction mixture was then poured into 10 mL ice/H2O. The product was isolated by vacuum filtration as brown crystals which were rinsed with a small amount of cold H2O and air dried. The crystals were further dried under vacuum (0.1 torr, 25° C.) to yield 173.4 mg (70.0% yield).

1. stirringto stir 1 h at 0° C.
2. customto come to room temperature
3. stirringstir overnight
4. customThe product was isolated by vacuum filtration as brown crystals which
5. washwere rinsed with a small amount of cold H2O and air
6. customdried
7. customThe crystals were further dried under vacuum (0.1 torr, 25° C.)
8. customto yield 173.4 mg (70.0% yield)