反应详情

To a solution of 21 mg (0.086 mmol) of 6,7difluoro-5-nitro-1,4-dihydroquinoxaline-2,3-dione in 0.5 mL of DMSO-d6 was added 16 mg (0.29 mmol) of sodium methoxide. The solution was shaken in a vortex for 10 s and kept at room temperature for 3 h. It was then added to 3 mL of water and acidified with 2 N HCl to pH=4. The precipitate was filtered, washed with water, and dried to leave a yellow solid (17 mg, 77%); mp 290-292° C.; 1H NMR (DMSO-d6), 3.899 (s, 3), 7.163 (1, d, J=11.6), 11.97 (mb, 1), 12.137 (s, 1). 19F NMR, −134.48 (mb). MS, 255 (M+, 100), 243 (15), 179 (16), 151 (40). HRMS, Calcd for C9HFN3O5 255.0287, found 255.0308.

1. waitkept at room temperature for 3 h
2. filtrationThe precipitate was filtered
3. washwashed with water
4. customdried