反应详情

温度

0 °C

To a solution of the alcohol from Step 1 (4.8 g, 14.7 mmol) and carbon tetrabromide (6.34 g, 19.1 mmol) in methylene chloride (100 mL) at 0° C. there was added, in portions, 1,2-bis(diphenylphosphino)ethane (6.34 g, 17.3 mmol). The mixture was stirred at 0° C. for 1 hour, and the solvent was evaporated. The residue was stirred in a mixture of ethyl acetate and water (150 mL each) for 30 minutes. After filtration, the organic portion of the filtrate was evaporated and the crude product purified by column chromatography on silica gel using 10% ethyl acetate in hexane as eluent to afford pure title compound as a yellow oil which solidified on standing.

1. customthe solvent was evaporated
2. stirringThe residue was stirred in a mixture of ethyl acetate and water (150 mL each) for 30 minutes
3. filtrationAfter filtration
4. customthe organic portion of the filtrate was evaporated
5. customthe crude product purified by column chromatography on silica gel using 10% ethyl acetate in hexane as eluent