反应详情

温度

50 °C

The 2× IPAc solution of (S)-Ethyl 2-amino-3-(4-(2-amino-6-((R)-1-(4-chloro-2-(3-methyl-1H-pyrazol-1-yl)phenyl)-2,2,2-trifluoroethoxy)pyrimidin-4-yl)phenyl)propanoate was added to a thin slurry of hippuric acid (6.49 g, 36 mol, 1.0 equiv.) in IPAc (208 mL, 10×) and EtOH (42 mL, 2×) at 60° C. The clear yellow solution was then cooled to 50° C., at which time seeding was added and stirred for 1 h at the same temperature. The suspension was then slowly cooled to room temperature and stirred for 14 h at room temperature. The solids were filtered, washed with ice-cold IPAc (0-5° C., 42 mL, 2×) and dried under vacuum at 50° C. overnight to afford a white solid (19.0 g, 69% yield). M.p.: 145° C. (DSC onset temperature)

1. additionwas added
2. temperatureThe suspension was then slowly cooled to room temperature
3. stirringstirred for 14 h at room temperature
4. filtrationThe solids were filtered
5. washwashed with ice-cold IPAc (0-5° C., 42 mL, 2×)
6. customdried under vacuum at 50° C. overnight