反应详情

温度

47.5 °C

Heat a mixture 7-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-6-yl trifluoromethanesulfonate (28.6 g, 84 mmol), dimethylformamide (74 mL) and glacial acetic acid (9.61 mL, 169 mmol) to 45° C. and then add 6.15% aqueous NaOCl (bleach, 612 g, 506 mmol) dropwise over 2 h. Heat at 45-50° C. for 2 h, cool to RT, collect the solids by filtration and wash with water (300 mL). Add DCM (200 mL) to the solids, cool the suspension in an ice-water bath and treat with a solution of 2.0 M N-methylamine in THF (126 mL, 253 mmol). Allow the mixture to slowly warm to RT and stir for 2 h. Remove the solvent under reduced pressure, treat with methanol (MeOH) (50 mL) and stir at RT for 30 min. Collect the solid by filtration and wash with MeOH. Treat the solid with EtOAc (30 mL) and stir at RT for 30 min. Collect the solid by filtration and wash with EtOAc to obtain the title compound (19.82 g, 73% yield). MS (m/z): 323.0 (M+1).

1. temperaturecool to RT
2. customcollect the solids
3. filtrationby filtration
4. washwash with water (300 mL)
5. temperatureAdd DCM (200 mL) to the solids, cool the suspension in an ice-water bath
6. temperatureAllow the mixture to slowly warm to RT
7. customRemove the solvent under reduced pressure
8. additiontreat with methanol (MeOH) (50 mL)
9. stirringstir at RT for 30 min
10. customCollect the solid
11. filtrationby filtration
12. washwash with MeOH
13. additionTreat the solid with EtOAc (30 mL)
14. stirringstir at RT for 30 min
15. customCollect the solid
16. filtrationby filtration
17. washwash with EtOAc