反应详情

To a mixture of 2-(4-cyanophenyl)-4-(4-fluorophenyl)-5-(4-pyridyl)-1H-imidazole (3.0 g, 8.7 mmol) [See Ex. 1 above] and K2CO3 (2.4 g, 17 mmol) in EtOH (120 mL) and H2O (6 mL) was added hydroxylamine hydrochloride (1.2 g, 17 mmol). After heating at reflux for 24 h, the reaction mixture was poured into H2O. The precipitate was collected, washed with H2O and air-dried. The crude product was dissolved in acetone, silica gel was added and the solvent was evaporated. The impregnated silica gel was added to the top of a flash column and the column was eluted with a solvent gradient of 2-10% MeOH/CHCl3 to afford the title compound as a white solid (3.0 g, 91%): ESMS (m/z): 374 (M++H).

1. temperatureAfter heating
2. temperatureat reflux for 24 h
3. customThe precipitate was collected
4. washwashed with H2O
5. customair-dried
6. dissolutionThe crude product was dissolved in acetone
7. additionsilica gel was added
8. customthe solvent was evaporated
9. additionThe impregnated silica gel was added to the top of a flash column
10. washthe column was eluted with a solvent gradient of 2-10% MeOH/CHCl3