反应详情

Dess-Martin reagent (1.75 g, 4.1 mmol) was added to a solution of diethyl{2-[2,3-difluoro-4-(5-fluoropyridin-2-yl)phenyl]-1,1-difluoro-2-hydroxyethyl}phosphonate (876 mg, 2.1 mmol) in methylene chloride (30 mL) at room temp—solution darkens to deep red over 1 hr. After stirring at rt for 1 hr, a solution of saturated aqueous sodium bicarbonate and saturated aqueous sodium thiosulfate (1:1) (ca. 20 mL) was added and the solution stirred until clear. The reaction mixture was extracted with dichloromethane, dried (sodium sulfate) and concentrated to afford diethyl {2-[2,3-difluoro-4-(5-fluoropyridin-2-yl)phenyl]-1,1-difluoro-2-oxoethyl}phosphonate as an off white solid which was used without further purification.

1. stirringthe solution stirred until clear
2. extractionThe reaction mixture was extracted with dichloromethane
3. dry with materialdried (sodium sulfate)
4. concentrationconcentrated