反应详情

温度

255 °C

A mixture of dimethyl[[6-(2-ethylbutyramido)-4-quinazolinylamino]methylene]propanedioate (5.3 g) and diphenyl ether (32 ml) was heated at 255° C. for 15 minutes and cooled to ambient temperature. Hexane was added to the reaction mixture. The resulting crystals were filtered off, washed with hexane and dried. The crude crystals were dissolved in a mixture of chloroform and methanol (10:1) under heating. Insoluble materials were removed by filtration. The filtrate was concentrated under reduced pressure to give crystals, which were recrystallized from a mixture of chloroform and hexane to give methyl 4-oxo-10-(2-ethylbutyramido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate (3.81 g).

1. temperaturecooled to ambient temperature
2. filtrationThe resulting crystals were filtered off
3. washwashed with hexane
4. customdried
5. dissolutionThe crude crystals were dissolved in a mixture of chloroform and methanol (10:1)
6. temperatureunder heating
7. customInsoluble materials were removed by filtration
8. concentrationThe filtrate was concentrated under reduced pressure
9. customto give crystals, which
10. customwere recrystallized from a mixture of chloroform and hexane