反应详情

温度

255 °C

A mixture of dimethyl [[6-(2,3-dimethylpentanamido)-4-quinazolinylamino]methylene]propanedioate (5.75 g) in diphenyl ether (28 ml) was stirred at 255° C. for 15 minutes and cooled to ambient temperature. The resulting solid was collected by filtration, washed with hexane, and dried. The crude crystals were chromatographed on silica gel with 4% methanol-chloroform. The product was recrystallized from a mixture of methanol and chloroform. There was obtained methyl 4-oxo-10-(2,3-dimethylpentanamido)-4H-pyrimido[1,2-C]quinazoline-3-carboxylate (0.4 g). Concentration of the mother liquor gave a crystalline residue, which was recrystallized from a mixture of chloroform and hexane to give additional 4.25 g of the same product.

1. temperaturecooled to ambient temperature
2. filtrationThe resulting solid was collected by filtration
3. washwashed with hexane
4. customdried
5. customThe crude crystals were chromatographed on silica gel with 4% methanol-chloroform
6. customThe product was recrystallized from a mixture of methanol and chloroform