反应详情

温度

50 °C

A mixture of 115e (40.0 g, 106 mmol), oxetan-3-one (11.4 g, 159 mmol), NaBH3CN (10.0 g, 159 mmol), and zinc chloride (21.3 g, 159 mmol) in methanol (700 mL) was stirred at 50° C. for 5 hours. water (50 mL) was added to the mixture and concentrated under reduced pressure. The residue was extracted with dichloromethane (3×200 mL) and the combined organic layer was concentrated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 40:1 dichloromethane/methanol to afford 115f (35 g, 73%). MS: [M+H]+ 434.

1. concentrationconcentrated under reduced pressure
2. extractionThe residue was extracted with dichloromethane (3×200 mL)
3. concentrationthe combined organic layer was concentrated under reduced pressure
4. customThe residue was purified by silica-gel column chromatography
5. washeluting with 40:1 dichloromethane/methanol