反应详情

4c (213 mg, 0.82 mmol) was refluxed in phosphorus oxychloride (5 mL) for 1 hour. The mixture was cooled to room temperature, concentrated, and diluted with saturated aqueous NaHCO3 and EtOAc. The aqueous layer was extracted with EtOAc, and the combined organic layers were dried over MgSO4, filtered, and concentrated. The residue was purified by silica gel chromatography (50-100% EtOAc in hexanes) to give the desired product, 4d.

1. concentrationconcentrated
2. additiondiluted with saturated aqueous NaHCO3 and EtOAc
3. extractionThe aqueous layer was extracted with EtOAc
4. dry with materialthe combined organic layers were dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by silica gel chromatography (50-100% EtOAc in hexanes)