反应详情

温度

110 °C

A mixture of (±)-3-[7-chloro-3-(4-methoxy-phenyl)-4-methyl-2-oxo-3,4-dihydro-2H-pyrimido[4,5-d]pyrimidin-1-yl]-benzonitrile (1.00 g; 2.42 mmol) (from Example 2 supra) and acetic acid 2-(3-amino-phenyl)-ethyl ester (2.03 g; 11.3 mmol) (from Example 3b supra) was heated in an oil bath at 110° C. for 1.5 hours. Upon cooling, the mixture was triturated with hexanes containing a small volume of ethyl acetate. The supernatant was decanted away and the residue was purified, in two runs, by flash chromatography (Biotage 40M; 50:50 to 70:30 ethyl acetate-hexanes gradient). The purified material was crystallized from ethyl acetate-hexanes to give (±)-acetic acid 2-{3-[8-(3-cyano-phenyl)-6-(4-methoxy-phenyl)-5-methyl-7-oxo-5,6,7,8-tetrahydro-pyrimido[4,5-d]pyrimidin-2-ylamino]-phenyl}-ethyl ester as a white solid. (1.03 g; 77.5%). Melting Point: 170–172° C.

1. temperatureUpon cooling
2. customthe mixture was triturated with hexanes containing a small volume of ethyl acetate
3. customThe supernatant was decanted away
4. customthe residue was purified, in two runs, by flash chromatography (Biotage 40M; 50:50 to 70:30 ethyl acetate-hexanes gradient)
5. customThe purified material was crystallized from ethyl acetate-hexanes