反应详情

温度

110 °C

(±)-3-[7-Chloro-3-(2-fluoro-4-methoxy-phenyl)-4-methyl-2-oxo-3,4-dihydro-2H-pyrimido[4,5-d]pyrimidin-1-yl]-benzonitrile (1.03 g; 2.42 mmol) (from Example 9a supra) was combined with aniline (1.00 mL; 10.97 mmol) (Aldrich) and heated at 110° C. for 1 hour. At this point, the reaction mixture was a solid mass. Methanol (75 mL) was added and the mixture was heated at 110° C. for 20 minutes with vigorous stirring (solid remained insoluble). Upon cooling, the solid was collected, washed with methanol and then ether and dried under high vacuum to give (±)-3-[3-(2-fluoro-4-methoxy-phenyl)-4-methyl-2-oxo-7-phenylamino-3,4-dihydro-2H-pyrimido[4,5-d]pyrimidin-1-yl]-benzonitrile. (Yield 1.00 g; 85.6%). A portion of this material was recrystallized from dichloromethane-ether-petroleum ether for characterization and testing. (Yield 0.22 g).

1. temperaturethe mixture was heated at 110° C. for 20 minutes
2. temperatureUpon cooling
3. customthe solid was collected
4. washwashed with methanol
5. dry with materialether and dried under high vacuum