反应详情

温度

255 °C

A mixture of dimethyl [[6-(2-methylpropionamido)-4-quinazolinylamino]methylene]propanedioate (8.4 g) in diphenyl ether (42 ml) was stirred at 255° C. for 15 minutes. The reaction mixture was cooled to ambient temperature to give crystals which were filtered off, washed with hexane and dried. There were obtained 6.9 g of the crude crystals. The crude crystals were dissolved in a mixture of chloroform and methanol (4:1) under heating. Insoluble materials were removed by filtration. The filtrate was concentrated under reduced pressure to about 150 ml. After cooling, there was obtained crystalline methyl 4-oxo-10-(2-methylpropionamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate (5.85 g).

1. temperatureThe reaction mixture was cooled to ambient temperature
2. customto give crystals which
3. filtrationwere filtered off
4. washwashed with hexane
5. customdried
6. customThere were obtained 6.9 g of the crude crystals
7. temperatureunder heating
8. customInsoluble materials were removed by filtration
9. concentrationThe filtrate was concentrated under reduced pressure to about 150 ml
10. temperatureAfter cooling