HRID1514443

反应详情

EQUATION

反应方程式

HRID 1514443 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-(2,4-Dimethyl-thiazol-5-yl)-1H-pyrimidin-2-one (120 mg, 0.58 mmol) in dry DMF (21 ml), 60% NaH (24 mg, 0.75 mmol) was added portionwise under inert atmosphere. After heating the mixture at 100° C. for 1 hour, 1-bromo-4-chloro-butane (86 μl, 0.75 mmol) was added at room temperature and the mixture was stirred overnight then was heated at 69° C. for 2 hours. 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 give 80 mg of the title compound as a solid (48% yield).

WORKUP

后处理

  1. temperaturethen was heated at 69° C. for 2 hours
  2. extractionthe mixture extracted with diethyl ether
  3. customto remove the dialkylated product
  4. washEthyl acetate was washed with brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated