反应详情

A suspension of [3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-thiourea (48 mg, 0.18 mmol) and of crude 6-bromo-2-(4-trifluoromethoxyl-phenyl)-cyclohexanone (65 mg, 0.19 mmol) in ethanol (2 mL) was heated to reflux under an atmosphere of nitrogen for 2 days. After cooling to room temperature the solvent was evaporated under reduced pressure and the residue was purified by reversed preparative HPLC using acetonitril/water (0.1% formic acid) to yield the title compound (16 mg, 17%) as a pale-brown oil. MS ISP (m/e): 501.0 (100) [(M+H)+]. 1H NMR (CDCl3, 300 MHz): δ (ppm)=7.61 (s, 1H), 7.35 (s, 1H), 7.08-7.20 (m, 4H), 6.82 (s, 1H), 6.65 (d, 1H), 4.06 (m, 1H), 3.56 (s, 3H), 2.75 (m, 2H), 2.28 (s, 3H), 2.25 (m, 1H), 1.77-1.98 (m, 3H).

1. temperatureto reflux under an atmosphere of nitrogen for 2 days
2. customwas evaporated under reduced pressure
3. customthe residue was purified by reversed preparative HPLC