反应详情

Alcohol 289 (1.75 g, 8.66 mmol) was treated with phosphorous tribromide (5.0 mL, 53 mmol) and the mixture was heated for 5 min, until the solid had melted and re-solidified. The mixture was cooled, treated with ice and partitioned between saturated aqueous sodium bicarbonate and dichloromethane. The organic phase was collected, washed with saturated aqueous sodium bicarbonate and brine, dried (anhydrous MgSO4), filtered and concentrated. Silica gel chromatography of the residue (eluent DCM) provided title compound 290 (2.0 g, 7.6 mmol, 87% yield) as a colorless solid. MS (M+H): 266.0

1. temperaturethe mixture was heated for 5 min, until the solid
2. temperatureThe mixture was cooled
3. additiontreated with ice
4. custompartitioned between saturated aqueous sodium bicarbonate and dichloromethane
5. customThe organic phase was collected
6. washwashed with saturated aqueous sodium bicarbonate and brine
7. dry with materialdried (anhydrous MgSO4)
8. filtrationfiltered
9. concentrationconcentrated