反应详情

To a solution of azido-(2-iodophenyl)-acetic acid methyl ester in THF (100 mL) is added triphenylphosphine (28.5 g, 109 mmol) in portions. The mixture is stirred at RT for 2 h then water (4 mL) is added and is heated to reflux. The solvent is removed under reduced pressure and ether (50 mL) is added followed by 2N HCl until acidic. The aqueous phase is washed with methylene chloride then is concentrated and basified with NaOH/ice until pH 12. The mixture is extracted with methylene chloride (3×200 mL) and the combined organic phases are dried over sodium sulfate. The solvent is removed under reduced pressure to give the title compound.

1. temperatureis heated to reflux
2. customThe solvent is removed under reduced pressure and ether (50 mL)
3. additionis added
4. washThe aqueous phase is washed with methylene chloride
5. concentrationthen is concentrated
6. extractionThe mixture is extracted with methylene chloride (3×200 mL)
7. dry with materialthe combined organic phases are dried over sodium sulfate
8. customThe solvent is removed under reduced pressure