HRID485657
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
5-Bromo-2-(4-aminobutyl)-3-methylpyridine, (0.875 g) and 5-(4-hydroxybenzyl)-2-methylthio-4-pyrimidone (0.745 g) were refluxed in pyridine (3 ml) for 24 hours. The pyridine was evaporated in vacuo. Residual pyridine was removed from the residue by azeotroping with water in vacuo and dried by azeotroping with ethanol. Water (20 ml) was added and the pH lowered to 6 with dilute hydrochloric acid. The solid obtained was recrystallised from ethanol/water, dimethylformamide/water and finally acetic acid/water to give 2-[4-(5-bromo-3-methylpyrid-2-yl)butylamino]-5-(4-hydroxybenzyl)-4-pyrimidone (0.54 g) m.p. 232°-4° C.
WORKUP
后处理
- customThe pyridine was evaporated in vacuo
- customResidual pyridine was removed from the residue
- customby azeotroping with water in vacuo
- customdried
- customby azeotroping with ethanol
- additionWater (20 ml) was added
- customThe solid obtained
- customwas recrystallised from ethanol/water, dimethylformamide/water and finally acetic acid/water