反应详情

温度

50 °C

A mixture of (S)-5-bromo-1-methyl-3-(5-(2-methylpiperazin-1-yl)pyridin-2-ylamino)pyridin-2(1H)-one 191h (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. The mixture was added to water (100 mL) and concentrated under reduced pressure. The residue was extracted with dichloromethane (200 mL×3). The combined organic layer was concentrated under reduced pressure and the residue was purified by silica-gel column chromatography eluting with 40:1 dichloromethane/methanol to afford 191i (35 g, 73%). MS: [M+H]+ 434.

1. concentrationconcentrated under reduced pressure
2. extractionThe residue was extracted with dichloromethane (200 mL×3)
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