反应详情

温度

60 °C

Combine 5-chloro-6-fluoro-8-methylpyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (5.00 g, 21.8 mmol), (S)-(2,2-dimethyl-1,3-dioxolan-4-yl)methyl-4-nitrobenzenesulfonate (7.60 g, 24.0 mmol), and N-methylpyrrolidinone (25.0 mL, 259 mmol). Add 1,8-Diazabicyclo[5.4.0]undec-7-ene (3.58 mL, 24.0 mmol) to the suspension. Heat to 60° C. and stir overnight. Add isopropyl acetate (50.0 mL, 427 mmol) followed by water (50.0 mL, 2780 mmol) while maintaining the temperature above 50° C. Stir at 60° C. for 1 hour, separate the phases and transfer the aqueous phase to a flask. Add isopropyl acetate (50.0 mL, 427 mmol) to the flask and stir at 60° C. for 1 hour and then separate the layers. Combine the organic phases and concentrate under vacuum to about 25 mL to give a solid. Cool to ambient temperature and stir for no longer than 2 hours, collect the solid by filtration, dry under vacuum overnight to give the title compound.

1. temperaturewhile maintaining the temperature above 50° C
2. stirringStir at 60° C. for 1 hour
3. customseparate the phases
4. customseparate the layers
5. concentrationCombine the organic phases and concentrate under vacuum to about 25 mL
6. customto give a solid
7. temperatureCool to ambient temperature
8. stirringstir for no longer than 2 hours
9. customcollect the solid
10. filtrationby filtration
11. customdry under vacuum overnight