HRID1514414

反应详情

EQUATION

反应方程式

HRID 1514414 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionthe mixture extracted with diethyl ether
  2. customto remove the dialkylated product
  3. washEthyl acetate was washed with brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated
  6. customThe residue was triturated with petroleum ether