反应详情

To a solution of the azide (11-4) of Example 52 in THF/water (80 ml/5 ml) (7.8 g, 40.6 mmol) was added triphenylphosphine (12.8 g, 48.72 mmol). The reaction mixture was stirred overnight at room temperature. The solvent was removed to dryness and the remaining residue was diluted with 100 ml 1N HCl and 100 ml water. The aqueous layer was extracted several times with dichloromethane. The aqueous layer was made basic (pH˜9) with an alkaline resin (Bio Rad AG 1-X8). The resin was filtered and washed thoroughly with water. The combined washings were dried under reduced pressure to give a white solid (6.60 g).

1. customThe solvent was removed to dryness
2. additionthe remaining residue was diluted with 100 ml 1N HCl and 100 ml water
3. extractionThe aqueous layer was extracted several times with dichloromethane
4. filtrationThe resin was filtered
5. washwashed thoroughly with water
6. customThe combined washings were dried under reduced pressure