Triethylamine → 1,3-dimethyl-6-[4-(3-[3-nitrophenoxy]propyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione

関与物質

反応手順

In 20 ml of dioxane were dissolved 1.69 g of the above oily compound 39, 1.12 g of 1,3-dimethyl-6-(1-piperazinyl)-2,4(1H,3H)-pyrimidinedione (compound 37) and 1 ml of triethylamine, and the solution was then heated under reflux for 4 hours to perform reaction. After completion of the reaction, insoluble matters were removed from the reaction mixture by filtration, the resulting filtrate was then concentrated. The residue (concentrate) was dissolved in chloroform, and the resulting chloroform solution was then washed with water. Afterward, the water-washed organic layer was dried over anhydrous magnesium sulfate and then treated under reduced pressure to distill off the solvent. Furthermore, the residue was purified through a silica gel column chromatograph (chloroform/methanol=100/1 to 25/1 in terms of volume ratio), and the purified material was then recrystallized from methanol. Afterward, the crystals were collected by filtration, washed and dried in order to obtain 1.35 g of 1,3-dimethyl-6-{4-[3-(3-nitrophenoxy)propyl]piperazin-1-yl}-2,4(1H,3 H)-pyrimidinedione.

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