反应详情

温度

80 °C

To a solution of 20 mg (0.082 mmol) of 6,7-difluoro-5-nitro-1,4-dihydroquinoxaline-2,3-dione in 0.5 m; of DMSO-d6 was added 2 drops of 30% ammonium hydroxide and the solution was heated at 80° C. for 24 h. To the mixture was added one more drop of 30% ammonium hydroxide and it was heated at 80° C. for 10 h. The mixture was added to 4 mL of water and then acidified with 2 N HCl to pH=1. The precipitate was filtered, washed with water, and dried to leave a yellow solid (15 mg, 76%); mp 250° C. (dec.); 1H NMR (DMSO-d6), 7.202 (1, d, J=11.5), 7.232 (sb, 2), 11.15 (mb, 1), 12.0 (mb, 1). 19F NMR, −133.84 (d, J=11.6). MS, 240 (M+, 100), 212 (10), 177 (10), 166 (20). HRMS, Calcd for CH5FN4O4 240.0290, found 240.0294.

1. temperaturewas heated at 80° C. for 10 h
2. filtrationThe precipitate was filtered
3. washwashed with water
4. customdried