反应详情

To a mixture of the ketone from Step 1 (10 g, 48 mmol) and Aliquat® 336 (20 mL) in CCl4 (40 mL) and toluene (80 mL) at r.t. was added NaOH pellets (3.8 g, 96 mmol). While stirring vigourously, the mixture was heated briefly to reflux and was then stirred overnight at r.t. After partitioning between CH2Cl2 and H2O, the whole was filtered through celite. The organic layer was dried (MgSO4), filtered, and evaporated. The residue was purified by flash chromatography (1:10 EtOAc:hexane) to give the title compound as a syrup (5.5 g).

1. temperaturethe mixture was heated briefly
2. temperatureto reflux
3. stirringwas then stirred overnight at r.t
4. customAfter partitioning between CH2Cl2 and H2O
5. filtrationthe whole was filtered through celite
6. dry with materialThe organic layer was dried (MgSO4)
7. filtrationfiltered
8. customevaporated
9. customThe residue was purified by flash chromatography (1:10 EtOAc:hexane)