反应详情

温度

110 °C

(±)-7-Chloro-3-(2-fluoro-4-methoxy-phenyl)-4-methyl-1-phenyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one (0.21 g; 0.53 mmol) (from Example 8c supra) and aniline (450 μL; 4.94 mmol) (Aldrich) were combined and heated at 110° C. for 1 hour. After cooling, the mixture was triturated with hexanes. The solid residue was dissolved in dichloromethane and washed with water and brine, dried over anhydrous sodium sulfate, filtered and concentrated. Purification by flash chromatography (Biotage 12M; 40:60 to 50:50 ethyl acetate-hexanes gradient) and then crystallization from dichloromethane-ether gave (±)-3-(2-fluoro-4-methoxy-phenyl)-4-methyl-1-phenyl-7-phenylamino-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one as a white solid. (Yield 0.20 g; 81.4%).

1. temperatureAfter cooling
2. customthe mixture was triturated with hexanes
3. dissolutionThe solid residue was dissolved in dichloromethane
4. washwashed with water and brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification by flash chromatography (Biotage 12M; 40:60 to 50:50 ethyl acetate-hexanes gradient)
9. customcrystallization from dichloromethane-ether