反应详情

bi) To a solution of rac-2-(4-fluoro-phenyl)-cyclohexanol (3.8 g, 20 mmol) in DCM (320 mL) was added Dess-Martin periodinane [1,1,1-tris(acetyloxy)-1,1-dihydro-1,2-benziodoxol-3-(1H)-one](10 g, 24 mmol) at room temperature and after 2 h the reaction mixture was washed with sodium hydrogen carbonate (10%, 150 mL). The organic phase was then separated and washed with sodium thiosulfite (10%, 150 mL) and then dried over sodium sulfate, filtered and evaporated. Purification by chromatography through silica gel, eluting with ethyl acetate:hexane (1:4) afforded the title compound (3.4 g, 89%) as white crystals. MS: m/e=192.1 (M).

1. washafter 2 h the reaction mixture was washed with sodium hydrogen carbonate (10%, 150 mL)
2. customThe organic phase was then separated
3. washwashed with sodium thiosulfite (10%, 150 mL)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customevaporated
7. customPurification by chromatography through silica gel
8. washeluting with ethyl acetate:hexane (1:4)