Piperazine → 3-Methylbenzylpiperazine

HRID 893286Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 893286
Br[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[CH:4]=1.[NH:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1>C1C=CC=CC=1.C(OCC)C>[CH3:9][C:5]1[CH:4]=[C:3]([CH:8]=[CH:7][CH:6]=1)[CH2:2][N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1

Komponenten

5

Edukt 2

HCID 4837PiperazineHCID 12099m-Xylyl bromide

Produkt 1

HCID 792133-MethylbenzylpiperazineAusbeute 78,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 241BenzeneLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

α-Bromo-m-xylene (10 ml, 74 mmole) was added to a solution of 75 g (11.8 equiv.) of anhydrous piperazine in 500 ml of benzene and the reaction was heated to reflux for two hours. After cooling to room temperature, the reaction was diluted with 300 ml of diethyl ether and washed with 500 ml of 0.2 M sodium hydroxide followed by two 500 ml portions of water. The organic solution was dried over sodium sulfate and the solvent removed to give 11.0 g (78%) of crude 1-(3-methylbenzyl)piperazine as a colorless oil.

Aufarbeitung

  1. temperaturethe reaction was heated
  2. temperatureto reflux for two hours
  3. washwashed with 500 ml of 0.2 M sodium hydroxide
  4. dry with materialThe organic solution was dried over sodium sulfate
  5. customthe solvent removed

Quellen und Nachweise

ORD-Eintrag
ord-c6e0b8d02e2348fcb55532b1fe88386d
Quelldatensatz
uspto-grants-1992_06
Patentnummer
US05124330

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