反应详情

The titled compound (Intermediate 5), was obtained by refluxing a suspension of Intermediate 4 (0.3 g, 1.684 mmol) in phosphorus oxychloride (ALDRICH, 1.88 mL, 20.2 mmol) for 2 h and then, adding the reaction mixture slowly to a mixture of water and ice. The solution was neutralized with solid Na2CO3 and extracted with DCM (25 mL). The aqueous layer was further extracted with DCM (2×5 mL) and the combined organic layers were washed with water (20 mL), then with brine (20 mL), and then dried over MgSO4. Solvent was removed under reduced pressure and the crude product was purified (silica gel column, eluting with Hexane/EtOAc mixtures from 100:0 to 40:60%) to obtain Intermediate 5 as a white solid.

1. temperatureby refluxing
2. additionadding the reaction mixture
3. extractionextracted with DCM (25 mL)
4. extractionThe aqueous layer was further extracted with DCM (2×5 mL)
5. washthe combined organic layers were washed with water (20 mL)
6. dry with materialwith brine (20 mL), and then dried over MgSO4
7. customSolvent was removed under reduced pressure
8. customthe crude product was purified
9. wash(silica gel column, eluting with Hexane/EtOAc mixtures from 100:0 to 40:60%)