反应详情

5-Bromo-2-(4-aminobutyl)-3-aminopyridine (0.5 g) and 2-nitroamino-5-(6-methylpyrid-3-ylmethyl)-4-pyrimidone (0.59 g) were refluxed in pyridine (2 ml) under nitrogen for 9 hours. The pyridine was removed in vacuo and the residual pyridine removed by azeotroping with n-propanol. After chromatography on silica in ethylacetate/ethanol/0.880 ammonia (15:10:2), the residue was crystallised from ethanol-ether and water (2 drops) to give 2-[4-(5-bromo-3-aminopyrid-2-yl)butylamino]-5-(6-methylpyrid-3-ylmethyl) 4-pyrimidone (0.52 g), m.p. 196°-197° C.

1. customThe pyridine was removed in vacuo
2. customthe residual pyridine removed
3. customby azeotroping with n-propanol
4. customAfter chromatography on silica in ethylacetate/ethanol/0.880 ammonia (15:10:2), the residue was crystallised from ethanol-ether and water (2 drops)