Potassium Carbonate → 1-Methyl-4-(2-nitrobenzyl)piperazine

HRID 372589

Reaktionsgleichung

Reaktionsgleichung von HRID 372589
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C(=O)([O-])[O-].[K+].[K+].[N+:14]([C:17]1[CH:24]=[CH:23][CH:22]=[CH:21][C:18]=1[CH2:19]Cl)([O-:16])=[O:15]>C(O)C>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:19][C:18]2[CH:21]=[CH:22][CH:23]=[CH:24][C:17]=2[N+:14]([O-:16])=[O:15])[CH2:4][CH2:3]1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 119212-Nitrobenzyl chlorideHCID 531671-Methylpiperazine

Produkt 1

HCID 7913741-Methyl-4-(2-nitrobenzyl)piperazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

In 20 volume parts of ethanol is dissolved 2.16 parts of o-nitrobenzyl chloride, followed by the addition of 1.02 parts of N-methyl piperazine and 1.3 parts of potassium carbonate. The mixture is reacted under reflux for 1 hour. The reaction mixture is then filtered and the solvent is removed from the filtrate by distillation under reduced pressure. The residue is extracted with water-ether (1:1). The ethereal layer is taken and dried over anhydrous sodium sulfate and the solvent is then distilled off. This procedure gives N1 -methyl-N4 -(2-nitrobenzyl)piperazine as a brown colored oily substance. Infrared absorption spectrum (liquid film)cm-1 : 1610, 1538.

Aufarbeitung

  1. customThe mixture is reacted
  2. temperatureunder reflux for 1 hour
  3. filtrationThe reaction mixture is then filtered
  4. customthe solvent is removed from the filtrate by distillation under reduced pressure
  5. extractionThe residue is extracted with water-ether (1:1)
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationthe solvent is then distilled off

Quellen und Nachweise

ORD-Eintrag
ord-29a915ece91c450c872c51aa161cef8c
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04091220

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