HRID65149

反应详情

EQUATION

反应方程式

HRID 65149 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 6-(3,4-dimethoxyphenyl)-3-methyl-2,4(1H,3H)-pyrimidinedione (3.0 g) in N,N-dimethylformamide (30 ml) was added sodium hydride (60% in oil, 0.5 g). The mixture was heated at 60° C. with stirring for 20 minutes and cooled to 0° C. To the mixture was added n-propyl iodide (15 ml) with stirring, which was continued at 0° C. for 2 hours and at ambient temperature for 3 hours. After addition of water, the reaction mixture was extracted with ethyl acetate. The organic extract was washed with water, dried over magnesium sulfate and evaporated under reduced pressure. The residue was triturated with diisopropyl ether and the resulting precipitates were collected by filtration to give 6-(3,4-dimethoxyphenyl)-3-methyl-2-propoxy-4(3H)-pyrimidinone (1.15 g) as by-product.

WORKUP

后处理

  1. temperaturecooled to 0° C
  2. stirringwith stirring
  3. waitwhich was continued at 0° C. for 2 hours and at ambient temperature for 3 hours
  4. extractionthe reaction mixture was extracted with ethyl acetate
  5. extractionThe organic extract
  6. washwas washed with water
  7. dry with materialdried over magnesium sulfate
  8. customevaporated under reduced pressure
  9. customThe residue was triturated with diisopropyl ether
  10. customthe resulting precipitates
  11. filtrationwere collected by filtration