反应详情

温度

50 °C

A mixture of 197d (0.75 g, 2.1 mmol), oxetan-3-one (0.24 mL, 4.2 mmol), NaBH3CN (0.32 g, 5.1 mmol), and zinc chloride/diethyl ether (5.1 mL, 5.1 mmol) in methanol (30 mL) was stirred at 50° C. for 5 hours. The solid was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 10:1 dichloromethane/methanol to afford 197e (550 mg, 64%). MS-ESI: [M+H]+ 421.

1. customThe solid was removed by filtration
2. concentrationthe filtrate was concentrated under reduced pressure
3. customThe residue was purified by silica-gel column chromatography
4. washeluting with 10:1 dichloromethane/methanol