反应详情

A mixture of 1-amino-3-(3,4-dichlorophenyl)-3-methylbutan-2-one hydrobromide (900 mg, 2.75 mmol), 4-fluorophenyl isothiocyanate (464 mg, 3.029 mmol), and Et3N (570 uL, 4.13 mmol) in dry benzene (20 mL) was heated at reflux 6 h. The reaction mixture was concentrated under reduced pressure, diluted with acetic acid (9 mL) and then heated at reflux 5 h. After cooling to room temperature and concentrating, the crude product was purified by flash column chromatography to afford 5-(2-(3,4-dichlorophenyl)propan-2-yl)-1-(4-fluorophenyl)-1H-imidazole-2-thiol (370 mg). 1H NMR (400 MHz, CDCl3) δ 7.15 (m, 2H), 6.91 (m, 2H), 6.80 (m, 2H), 6.62 (m, 2H), 1.61 (s, 6H).

1. temperaturewas heated
2. temperatureat reflux 6 h
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additiondiluted with acetic acid (9 mL)
5. temperatureheated
6. temperatureat reflux 5 h
7. concentrationconcentrating
8. customthe crude product was purified by flash column chromatography