反应详情

To a solution of the tertiary alcohol from Step 2 (4.5 g, 20.1 mmol) in CH2Cl2 (100 mL), MeOH (100 mL) and H2O (25 mL) was added Oxone® (9 g). After 3 h at r.t. a second 9 g portion of Oxone® was added and the mixture was stirred overnight at r.t. The solvent was then removed under vacuum, and the residue was partitioned between EtOAc and H2O. The organic phase was washed with H2O and brine, and was then dried (MgSO4), filtered, and evaporated. Purification was effected by flash chromatography (1:2 EtOAc: hexane) to give 5.5 g of the title compound as a tan coloured oil.

1. customThe solvent was then removed under vacuum
2. customthe residue was partitioned between EtOAc and H2O
3. washThe organic phase was washed with H2O and brine
4. dry with materialwas then dried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customPurification