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

HRID 1085249
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1085249
[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH2:8]Br)=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH3:12][N:13]1[C:18]([NH:19][CH2:20][CH2:21]CNC2C=CC([N+]([O-])=O)=CC=2)=[CH:17][C:16](=[O:33])[N:15]([CH3:34])[C:14]1=[O:35].[CH2:36]([N:38](CC)CC)[CH3:37]>C(O)(C)C>[CH3:12][N:13]1[C:18]([N:19]2[CH2:20][CH2:21][N:38]([CH2:8][C:7]3[CH:10]=[CH:11][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=3)[CH2:36][CH2:37]2)=[CH:17][C:16](=[O:33])[N:15]([CH3:34])[C:14]1=[O:35]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 660114-Nitrobenzyl bromideHCID 200612441,3-dimethyl-6-[3-(4-nitroanilino)propylamino]-2,4-(1H,3H)-pyrimidinedione2×

Produkt 1

HCID 104736221,3-dimethyl-6-[4-(4-nitrobenzyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776Isopropanol
Lösungsmittel

Versuchsvorschrift

First, 0.48 g of 4-nitrobenzyl bromide, 0.5 g of 1,3-dimethyl-6-(piperazin -1-yl)-2,4(1H,3H)-pyrimidinedione (compound 2) and 0.5 ml of triethylamine were suspended in 5 ml of isopropanol, and the resulting suspension was then heated under reflux for 8 hours. Afterward, the used solvent was removed from the resulting reaction mixture by distillation under reduced pressure, and the residue was dissolved in chloroform and was then washed with water. The washed organic layer was dried over anhydrous sodium sulfate. Furthermore, the dried organic layer was subjected to distillation under reduced pressure so as to remove the solvent therefrom, and the residue was then purified through a silica gel column chromatograph (chloroform/methanol=50/1 to 20/1 in terms of volume ratio) in order to obtain 0.88 g of 1,3-dimethyl-6-[4-(4-nitrobenzyl)piperazin-1-yl]-2,4(1H,3H)-pyrimidinedione.

Aufarbeitung

  1. temperaturethe resulting suspension was then heated
  2. temperatureunder reflux for 8 hours
  3. customAfterward, the used solvent was removed from the resulting reaction mixture by distillation under reduced pressure
  4. dissolutionthe residue was dissolved in chloroform
  5. washwas then washed with water
  6. dry with materialThe washed organic layer was dried over anhydrous sodium sulfate
  7. distillationFurthermore, the dried organic layer was subjected to distillation under reduced pressure so as
  8. customto remove the solvent
  9. customthe residue was then purified through a silica gel column chromatograph (chloroform/methanol=50/1 to 20/1 in terms of volume ratio) in order

Quellen und Nachweise

ORD-Eintrag
ord-744d1405421e4baca24789681da47d84
Quelldatensatz
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05008267

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