反应详情

To a solution of the acetate 176 (500 mg, 0.85 mmol) in CH2Cl2 (20 mL) were added AlCl3 (691 mg, 5.18 mmol) and acetyl chloride (0.37 mL, 5.18 mmol) at 0° C. The mixture was warmed up to rt slowly and left at rt for 3 hours. The mixture was cooled to 0° C. and added aq. 1N HCl solution to quench the reaction. The mixture was extracted with EtOAc (100 mL). The organic layer was washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by silica gel column chromatography to provide the product 177 (540 mg, quantitative yield).

1. temperatureThe mixture was cooled to 0° C.
2. customto quench
3. customthe reaction
4. extractionThe mixture was extracted with EtOAc (100 mL)
5. washThe organic layer was washed with brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe residue was purified by silica gel column chromatography