反应详情

To a solution of alcohol 105 (5.33 g, 8.01 mmol) in ether (50 mL) were added phosphorus tribromide (0.26 mL, 2.80 mmol) and catalytic amount of pyridine at 0° C. The mixture was allowed to warm to room temperature and stirred at room temperature for 15 hours. The mixture was extracted with EtOAc/H2O (100 mL/150 mL). The combined organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by silica gel column chromatography to provide the title bromide 106 (4.15 g, 71%).

1. extractionThe mixture was extracted with EtOAc/H2O (100 mL/150 mL)
2. dry with materialThe combined organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue was purified by silica gel column chromatography