反应详情

To a stirred suspension of (4-(4-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)benzyl)piperazin-1-yl)(3-nitrophenyl)methanone (1.730 mmol, 850 mg) and iron powder (17.30 mmol, 966 mg) in 2-propanol was added a small volume of hydrochloric acid (37%). The reaction was refluxed for 1 hour then was allowed to cool to room temperature. The reaction was diluted with dichloromethane and solid potassium carbonated was added. The reaction was stirred for 1 hour then was filtered through celite washing with dichloromethane. The filtrate was concentrated under reduced pressure. The crude material was chromatographed on silica eluting with ethyl acetate to give the title compound (440 mg). MS (ESI) m/z 462.2 [M+H]+

1. temperatureThe reaction was refluxed for 1 hour
2. additionwas added
3. filtrationthen was filtered
4. washthrough celite washing with dichloromethane
5. concentrationThe filtrate was concentrated under reduced pressure
6. customThe crude material was chromatographed on silica eluting with ethyl acetate