反应详情

Compound 3 (150 g, 704 mmol, 1 equiv) was suspended in a mixture of concentrated sulfuric acid (250 mL) and water (1.25 L). The mixture was refluxed overnight. The reaction was cooled and extracted with 1.5 L of dichloromethane. The organic layer was washed with saturated sodium bicarbonate (1.5 L), dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified over silica gel (800 g), eluting with heptanes to give compound 4 (95 g, 69% yield) as a light yellow oil.

1. temperatureThe mixture was refluxed overnight
2. temperatureThe reaction was cooled
3. extractionextracted with 1.5 L of dichloromethane
4. washThe organic layer was washed with saturated sodium bicarbonate (1.5 L)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified over silica gel (800 g)
8. washeluting with heptanes