HRID1514414
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
To a solution of 4-(6-methyl-pyridin-2-yl)-1H-pyrimidin-2-one (200 mg, 1.06 mmol) in dry DMF (20 ml), 60% NaH (55 mg, 1.39 mmol) was added portionwise. After heating the mixture at 100° C. for 1 hour, 1-bromo-4-chloro-butane (187 μl 1.39 mmol) was added and the mixture was stirred overnight at room temperature. Water was added and the mixture extracted with diethyl ether to remove the dialkylated product and finally with ethyl acetate. Ethyl acetate was washed with brine, dried (Na2SO4) and evaporated. The residue was triturated with petroleum ether to give 173 mg of the title compound as a solid (58% yield).
WORKUP
后处理
- extractionthe mixture extracted with diethyl ether
- customto remove the dialkylated product
- washEthyl acetate was washed with brine
- dry with materialdried (Na2SO4)
- customevaporated
- customThe residue was triturated with petroleum ether