反应详情

温度

25 °C

Add 5,7-dihydropyrido[2,3-d][3]benzazepin-6-one (33.8 g, 0.16 mol) in acetonitrile (340.0 mL) and stir at 20-30° C. for 0.5-1 hour. Add cesium carbonate (104.6 g, 0.32 mol) and (2-bromoethoxy)-tert-butyldimethylsilane (42.2 g, 0.18 mol) and heat the reaction mixture to 70-80° C. for 18-20 hours. Cool the reaction mixture to 20-25° C. and filter through diatomaceous earth (50.6 g). Wash the filter cake with acetonitrile (2×50.6 mL) and concentrate the filtrate under reduced pressure to arrive at a total volume of approximately 67.5 mL. Add toluene (152 mL), active carbon (2.53 g) and heat the mixture to 60-70° C. for 1-2 hours. Cool the mixture to 25-35° C. and filter the reaction mixture over diatomaceous earth (50.6 g). Rinse the filter cake with toluene (17.0 mL) and concentrate under reduced pressure to obtain the title compound as a light brown oil that crystallizes on standing (56.8 g, 92.2%).

1. temperatureCool the reaction mixture to 20-25° C.
2. filtrationfilter through diatomaceous earth (50.6 g)
3. washWash the filter cake with acetonitrile (2×50.6 mL)
4. concentrationconcentrate the filtrate under reduced pressure
5. temperatureAdd toluene (152 mL), active carbon (2.53 g) and heat the mixture to 60-70° C. for 1-2 hours
6. temperatureCool the mixture to 25-35° C.
7. filtrationfilter the reaction mixture over diatomaceous earth (50.6 g)
8. washRinse the filter cake with toluene (17.0 mL)
9. concentrationconcentrate under reduced pressure