反应详情

温度

80 °C

Palladium on activated carbon (0.4 g, 10% w/w) was added to a suspension of (R)-5-(2-azido-1-(tert-butyldimethylsilyloxy)ethyl)-8-(benzyloxy)quinolin-2(1H)-one (2.05 g, 4.60 mmol) and ammonium formate (2.87 g, 63 mmol) in methanol (50 mL). The reaction mixture was heated at 80° C. for 1 hour. If after this time, the reaction had not reached completion; the reaction mixture was filtered through celite, washing with methanol. The reaction mixture was concentrated to approximately 50 mL then ammonium formate (2.87 g, 63.0 mmol) and Palladium on activated carbon (0.40 g, 10% w/w) were added. The reaction mixture was heated at 80° C. for 20 minutes, and then filtered through celite, washing with water. The reaction mixture was concentrated under reduced pressure. The resulting solid was washed with water, triturated with ethyl acetate and collected by filtration to afford the title compound (1.32 g, 86%).

1. filtrationthe reaction mixture was filtered through celite
2. washwashing with methanol
3. concentrationThe reaction mixture was concentrated to approximately 50 mL
4. temperatureThe reaction mixture was heated at 80° C. for 20 minutes
5. filtrationfiltered through celite
6. washwashing with water
7. concentrationThe reaction mixture was concentrated under reduced pressure
8. washThe resulting solid was washed with water
9. customtriturated with ethyl acetate
10. filtrationcollected by filtration