反应详情

A solution of the product from Example 311b (0.73 g, 2.309 mmol) in dichloromethane (11.55 mL) under nitrogen was treated dropwise with tribromophosphine (0.218 mL, 2.309 mmol), stirred for one hour at ambient temperature and poured into ice water and the pH was adjusted to pH 9 by addition of solid sodium bicarbonate added portionwise. An emulsion formed that was partially removed by filtration. The aqueous layer was extracted with dichloromethane and the organics were combined, washed with saturated aqueous sodium chloride, dried (Na2SO4) filtered, and concentrated to afford the title compound (0.75 g, 86%).

1. additionadded portionwise
2. customAn emulsion formed
3. customthat was partially removed by filtration
4. extractionThe aqueous layer was extracted with dichloromethane
5. washwashed with saturated aqueous sodium chloride
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated