HRID1514410

反应详情

EQUATION

反应方程式

HRID 1514410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 5-methyl-4-pyridin-3-yl-1H-pyrimidin-2-one (100 mg, 0.53 mmol) in DMSO (2 ml), 60% NaH (23 mg, 0.59 mmol) was added portionwise. After heating the mixture at 60° C. for 1 hour, 1-bromo-4-chloro-butane (100 mg, 0.59 mmol) dissolved in DMSO (0.8 ml) was added at 60° C. and the heating was maintained for further 2 hours. After cooling to 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 to afford 100 mg of the title compound as yellow oil (68% yield).

WORKUP

后处理

  1. additionwas added at 60° C.
  2. temperaturethe heating was maintained for further 2 hours
  3. temperatureAfter cooling to room temperature
  4. extractionthe mixture extracted with diethyl ether
  5. customto remove the dialkylated product
  6. washEthyl acetate was washed with brine
  7. dry with materialdried (Na2SO4)
  8. customevaporated