HRID1729313

反应详情

EQUATION

反应方程式

HRID 1729313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.3 g of 1-(3-phenyloxypropyl)piperazine and 0.5 g of 6-chloro-1-methyl-2,4(1H,3H)-pyrimidinedione were dissolved in 15 ml of isopropanol, and 2.7 ml of triethylamine was then added. Next, the solution was heated under reflux with stirring for 12 hours and then allowed to stand for cooling, and the solvent was distilled off. The resultant residue was dissolved in 100 ml of chloroform. The chloroform layer was washed with water, dried over anhydrous sodium sulfate and then concentrated under reduced pressure to obtain an oily product. This oily product was purified through a silica gel column chromatograph (chloroform/methanol=30/1 in volume ratio), thereby obtaining 0.73 g of 1-methyl-6-[4-(3-phenoxypropyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione.

WORKUP

后处理

  1. temperatureNext, the solution was heated
  2. temperatureunder reflux
  3. temperaturefor cooling
  4. distillationthe solvent was distilled off
  5. dissolutionThe resultant residue was dissolved in 100 ml of chloroform
  6. washThe chloroform layer was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customto obtain an oily product
  10. customThis oily product was purified through a silica gel column chromatograph (chloroform/methanol=30/1 in volume ratio)