反应详情

To a solution of N-(4,4-difluorocyclohexyl)-8-nitroquinazolin-4-amine (90 mg, 0.292 mmol) in EtOH (2 mL) were added iron powder (163 mg, 2.92 mmol) and NH4Cl (127 mg, 2.33 mmol) and the reaction mixture was heated at reflux for 2 h. Then the reaction mixture was filtered through celite. The celite bed was washed with 10% MeOH in CHCl3. The filtrate was washed with a saturated aq. NaHCO3 solution and water. The organic layer was separated, dried, filtered and concentrated to afford 70 mg of the title product. 1H NMR (300 MHz, DMSO d6): δ 8.38 (s, 1H), 7.64 (d, J=7.2 Hz, 1H), 7.35 (d, J=7.8 Hz, 1H), 7.19-7.14 (t, J=7.8 Hz, 1H), 6.87 (d, J=7.8 Hz, 1H), 5.71 (s, 2H), 4.38 (m, 1H), 2.09-1.97 (m, 6H), 1.73-1.69 (m, 2H); MS (m/z): 279.12 (M+H)+.

1. temperaturethe reaction mixture was heated
2. temperatureat reflux for 2 h
3. filtrationThen the reaction mixture was filtered through celite
4. washThe celite bed was washed with 10% MeOH in CHCl3
5. washThe filtrate was washed with a saturated aq. NaHCO3 solution and water
6. customThe organic layer was separated
7. customdried
8. filtrationfiltered
9. concentrationconcentrated