Reaktion #1172436

Reaktionsgleichung

above oily compound 39

1,3-dimethyl-6-{N-(2-phenylethyl)-2-[3-(4-nitrophenyl)propylamino]ethylamino)-2,4-(1H,3H)-pyrimidinedione

1,3-dimethyl-6-(1-piperazinyl)-2,4(1H,3H)-pyrimidinedione

compound 37

1,3-dimethyl-6-(1-piperazinyl)-2,4(1H,3H)-pyrimidinedione

triethylamine

dioxane

→

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

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution was then heated
2. 2
   Temperaturunder reflux for 4 hours
3. 3
   Sonstigereaction
4. 4
   SonstigeAfter completion of the reaction, insoluble matters
5. 5
   Sonstigewere removed from the reaction mixture by filtration
6. 6
   Einengenthe resulting filtrate was then concentrated
7. 7
   EinengenThe residue (concentrate)
8. 8
   workup.DISSOLUTIONwas dissolved in chloroform
9. 9
   Waschenthe resulting chloroform solution was then washed with water
10. 10
    WaschenAfterward, the water-washed organic layer
11. 11
    Trocknenwas dried over anhydrous magnesium sulfate
12. 12
    workup.ADDITIONtreated under reduced pressure
13. 13
    workup.DISTILLATIONto distill off the solvent
14. 14
    SonstigeFurthermore, the residue was purified through a silica gel column chromatograph (chloroform/methanol=100/1 to 25/1 in terms of volume ratio)
15. 15
    Sonstigethe purified material was then recrystallized from methanol
16. 16
    FiltrationAfterward, the crystals were collected by filtration
17. 17
    Waschenwashed
18. 18
    Sonstigedried in order

Vorschrift

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.

Quelle