反应详情

To a solution of 9 (0.25 g, 1.29 mmol) and 5 (0.29 ml, 1.44 mmol) in EtOH (8 mL) were added 2 drops of conc. HCl. The mixture was heated under reflux overnight. After cooling to room temperature, EtOH was removed under reduced pressure. The residue was partitioned between sat. NaHCO3 (aq.) and EtOAc (100 mL each) and the aquous layer was extracted with EtOAc (2×50 mL). The combined organic layers were dried over MgSO4, the solids were filtered, and the filtrate was concentrated under reduced pressure. The residue was purified on Florisil® (50% EtOAc/Hexanes to 15% MeOH/EtOAc) to yield the title compound as a light yellow solid (0.25 g).

1. temperatureThe mixture was heated
2. temperatureunder reflux overnight
3. customEtOH was removed under reduced pressure
4. customThe residue was partitioned between sat. NaHCO3 (aq.) and EtOAc (100 mL each)
5. extractionthe aquous layer was extracted with EtOAc (2×50 mL)
6. dry with materialThe combined organic layers were dried over MgSO4
7. filtrationthe solids were filtered
8. concentrationthe filtrate was concentrated under reduced pressure
9. customThe residue was purified on Florisil® (50% EtOAc/Hexanes to 15% MeOH/EtOAc)