反应详情

A solution of 24 mg (0.098 mmol) of 6,7difluoro-5-nitro-1,4-dihydroquinoxaline-2,3-dione and 24 mg (0.33 mmol) of sodium ethoxide (96%) in 0.5 mL of DMSO-d6 was kept at room temperature for 5 h. The red solution was 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 (24 mg, 91%); mp 293-295° C.; 1H NMR (DMSO-d6), 1.239 (t, 3, J=7.0), 4.141 (q, 2, J=7.2), 7.152 (1, d, J=11.7), 11.975 (s, 1), 12.135 (s, 1). 19F NMR, −134.06 (mb). MS, 269 (M+, 90), 241 (100), 195 (70). HRMS, Calcd for C10H8FN3O5269.0443, found 269.0454.

1. filtrationThe precipitate was filtered
2. washwashed with water
3. customdried