反应详情

温度

50 °C

A mixture of 224b (2.3 g, 6.8 mmol), oxetan-3-one (1.4 g, 20.0 mmol), NaBH3CN (620 mg, 10 mmol), and zinc chloride (1.36 g, 10 mmol) in methanol (20 mL) was stirred at 50° C. for 3 hours. The mixture was added to water (40 mL) and concentrated under reduced pressure. The residue was extracted with dichloromethane three times. The combined organic layer was dried and concentrated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 50:1 dichloromethane/methanol to afford 224c (2.0 g, 75%). MS-ESI: [M+H]+ 391.2.

1. concentrationconcentrated under reduced pressure
2. extractionThe residue was extracted with dichloromethane three times
3. customThe combined organic layer was dried
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by silica-gel column chromatography
6. washeluting with 50:1 dichloromethane/methanol