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Triethylamine → 2-Nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]benzaldehyde

HRID 1649199
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1649199
[N+:1]([C:4]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)=[CH:8][C:5]=1[CH:6]=[O:7])([O-:3])=[O:2].C(N(CC)CC)C.[CH3:25][O:26][C:27]1[CH:28]=[C:29]([CH:33]=[CH:34][C:35]=1[O:36][CH3:37])[C:30](Cl)=[O:31]>CN(C=O)C>[N+:1]([C:4]1[CH:11]=[CH:10][C:9]([N:12]2[CH2:13][CH2:14][N:15]([C:30](=[O:31])[C:29]3[CH:33]=[CH:34][C:35]([O:36][CH3:37])=[C:27]([O:26][CH3:25])[CH:28]=3)[CH2:16][CH2:17]2)=[CH:8][C:5]=1[CH:6]=[O:7])([O-:3])=[O:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 77070Veratroyl chlorideHCID 109893842-Nitro-5-piperazinylbenzaldehyde

Produkt 1

HCID 132363012-Nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]benzaldehydeAusbeute 53 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

2-Nitro-5-piperazinylbenzaldehyde (5 g) was suspended in 50 ml of DMF and 6 ml of triethylamine was added to the suspension. A solution of 4.4 g of 3,4-dimethoxybenzoyl chloride in 20 ml of DMF was added dropwise thereto with ice cooling externally while stirring and the mixture was stirred at room temperature for 2 hours and poured into saturated saline and extracted with methylene chloride. After washing with water, the methylene chloride layer was dried over anhydrous sodium sulfate. Then, the solvent was removed by distillation and to the residue was added methyl alcohol and the mixture was heated and cooled and crystals which formed were recrystallized form DMF to give 4.5 g of 2-nitro-5-[4-(3,4-dimethoxybenzoyl)-1-piperazinyl]benzaldehyde, m.p. 196°-198° C., yellow crystal.

Aufarbeitung

  1. stirringthe mixture was stirred at room temperature for 2 hours
  2. additionpoured into saturated saline
  3. extractionextracted with methylene chloride
  4. washAfter washing with water
  5. dry with materialthe methylene chloride layer was dried over anhydrous sodium sulfate
  6. customThen, the solvent was removed by distillation and to the residue
  7. additionwas added methyl alcohol
  8. temperaturethe mixture was heated
  9. temperaturecooled
  10. customcrystals which formed
  11. customwere recrystallized form DMF

Quellen und Nachweise

ORD-Eintrag
ord-4d3ce01e8b304e919e6c0f6711038b89
Quelldatensatz
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04415572

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