反应详情

A mixture of 1-(5-bromo-2-fluorophenyl)-3-(tert-butyldimethylsilyloxy)-2,2-difluoropropan-1-ol (19.0 g, mmol) and Pyridinium dichromate (90.0 g, 239.2 mmol) in Dichloromethane (200 mL) was refluxed for 16 h under constant stirring. The catalyst was filtered through a pad of celite and the filtrate was concentrated under reduced pressure to obtain brown colored thick mass. Crude product was purified by column chromatography on silica gel with 1% ethyl acetate in Hexane to obtain title compound as colorless oil. Yield=17.0 g (90%). TLC (10% ethyl acetate in Hexane): Rf=0.56),

1. temperaturewas refluxed for 16 h under constant stirring
2. filtrationThe catalyst was filtered through a pad of celite
3. concentrationthe filtrate was concentrated under reduced pressure
4. customto obtain brown colored thick mass
5. customCrude product was purified by column chromatography on silica gel with 1% ethyl acetate in Hexane