反应详情

Dissolve 4-cyanophenacyl bromide (1.82 g, 8.14 mmol), (R)-(1-methyl-2,2,2-trifluoroethyl)-thiourea (1.4 g, 8.14 mmol) and sodium bicarbonate (0.68 g, 8.14 mmol) in absolute ethanol. Heat at reflux 2 h, cool to room temperature and let stand over 2 days. Filter and collect the resulting crude product as a tan solid. Purify by chromatography on silica gel (34 g) eluting with hexane/EtOAc (19:1 to 4:1 over 30 min, 4:1 over 10 min; 40 mL/min) to obtain the desired intermediate as a white solid (1.23 g, 52%). MS (ES+) m/z: 298 (M+H)+.

1. temperatureHeat
2. temperatureat reflux 2 h
3. filtrationFilter
4. customcollect the resulting crude product as a tan solid
5. customPurify by chromatography on silica gel (34 g)
6. washeluting with hexane/EtOAc (19:1 to 4:1 over 30 min, 4:1 over 10 min; 40 mL/min)