反应详情

In 20 ml of dioxane were suspended 2.76 g of N-(2-chloroethyl)benzamide, 1.12 g of 1,3-dimethyl-6-(1-piperazinyl)-2,4(1H,3H)-pyrimidinedione, 3.75 g of sodium iodide and 1.4 ml of triethylamine, and the solution was heated under reflux with stirring for 15 hours. Afterward, the solvent was distilled off, and the resultant residue was dissolved in chloroform, washed with water, and then concentrated to dryness. The residue was purified through a silica gel column chromatograph (chloroform/methanol=100/1 to 100/5 in volume ratio), thereby obtaining 1.25 g of the crystals of 1,3-dimethyl-6-[4-(N-benzoyl-2-aminoethyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione.

1. temperaturethe solution was heated
2. temperatureunder reflux
3. distillationAfterward, the solvent was distilled off
4. dissolutionthe resultant residue was dissolved in chloroform
5. washwashed with water
6. concentrationconcentrated to dryness
7. customThe residue was purified through a silica gel column chromatograph (chloroform/methanol=100/1 to 100/5 in volume ratio)