反应详情

A suspension of Intermediate 6 (0.660 g, 2.89 mmol) in phosphorus oxychloride (ALDRICH, 0.404 mL, 43.4 mmol) was heated under reflux for 2 h, the starting material dissolving during the process. The mixture was slowly added to a mixture of water and ice. The resulting 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 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 afford Intermediate 7 as a pale yellow solid.

1. temperaturewas heated
2. temperatureunder reflux for 2 h
3. dissolutionthe starting material dissolving during the process
4. extractionextracted with DCM (25 mL)
5. extractionThe aqueous layer was further extracted with DCM (2×5 mL)
6. washthe combined organic layers were washed with water (20 mL)
7. dry with materialthen with brine (20 mL), and dried over MgSO4
8. customSolvent was removed under reduced pressure
9. customthe crude product was purified
10. wash(silica gel column, eluting with Hexane/EtOAc mixtures from 100:0 to 40:60%)