反应详情

To a solution of [(1S,2S,3S,4R,5S)-2,3,4-tribenzyloxy-5-[4-chloro-3-[[4-(trifluoromethoxy)phenyl]methyl]phenyl]-6,8-dioxabicyclo[3.2.1]octan-1-yl]methanol 15o (0.7 g, 0.94 mmol) in ethyl acetate (30 mL) was added 2-iodoxybenzoic acid (0.79 g, 2.81 mmol) at room temperature. The mixture was refluxed for 24 hours and filtered. The filtrate was washed with saturated aqueous sodium bicarbonate (10 mL×2) and saturated aqueous sodium chloride (10 mL×2) in turn, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo to give the title compound 15p as yellow oil (0.71 g, 100%). This material was not further purified.

1. temperatureThe mixture was refluxed for 24 hours
2. filtrationfiltered
3. washThe filtrate was washed with saturated aqueous sodium bicarbonate (10 mL×2) and saturated aqueous sodium chloride (10 mL×2) in turn
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated in vacuo