反应详情

温度

60 °C

3-Benzyl-5-(2-fluoro-4-nitrophenylamino)-6,8-dimethylpyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (4.1 mg, 9.42 mmol), palladium hydroxide (20% on carbon, 4 g) and ammonium formate (4 g, 63.4 mmol) were stirred in dioxane (200 mL) at 90° C. for 4 hours in a sealed pressure vessel. The suspension was filtered and the solid refluxed in DMF (20 mL) for 1 hour then filtered. This was repeated 3 times. The filtrates were combined and evaporated. The residue was dissolved in DMF (50 mL) and Quadrapure palladium scavenger (20 g) was added and the mixture stirred at 60° C. overnight. The mixture was filtered and evaporated, ether was added and a precipitate formed. This solid was filtered to give 2 g of the title compound (67%). [M+H] calc'd for C15H14FN5O2, 316. found, 316.

1. filtrationThe suspension was filtered
2. temperaturethe solid refluxed in DMF (20 mL) for 1 hour
3. filtrationthen filtered
4. customevaporated
5. dissolutionThe residue was dissolved in DMF (50 mL)
6. additionQuadrapure palladium scavenger (20 g) was added
7. filtrationThe mixture was filtered
8. customevaporated
9. additionether was added
10. customa precipitate formed
11. filtrationThis solid was filtered