Glyoxal → 1,4-Diethylpiperazin-2-one

HRID 35731

Reaktionsgleichung

Reaktionsgleichung von HRID 35731
[CH:1]([CH:3]=O)=[O:2].[CH2:5]([NH:7][CH2:8][CH2:9][NH:10][CH2:11][CH3:12])[CH3:6]>O>[CH2:5]([N:7]1[CH2:8][CH2:9][N:10]([CH2:11][CH3:12])[CH2:3][C:1]1=[O:2])[CH3:6]

Komponenten

4

Edukt 2

HCID 7860GlyoxalHCID 67105N,N'-Diethylethylenediamine

Produkt 1

HCID 5813421,4-Diethylpiperazin-2-oneAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 10.0 g (69.0 mmoles) of 40 percent glyoxal and 200 ml of distilled water is rapidly added 8.0 g (69.0 mmoles) of N,N'-diethylethylenediamine. The solution is heated rapidly to reflux and heating maintained for 5 minutes. The dark brown solution is allowed to cool to room temperature and is then evaporated at 60° C. under water pump vacuum to a viscous brown oil. The oil is distilled in a short path distillation apparatus to yield 10 g (93 percent yield) of 1,4-diethylpiperazin-2-one in the form of a yellow oil. Purity is greater than 99 percent by capillary gas chromatograph.

Aufarbeitung

  1. temperatureThe solution is heated rapidly
  2. temperatureto reflux
  3. temperatureheating
  4. temperaturemaintained for 5 minutes
  5. customis then evaporated at 60° C. under water
  6. distillationThe oil is distilled in a short path distillation apparatus

Quellen und Nachweise

ORD-Eintrag
ord-433d5ac6e71b4bd88a7c285e92d673ec
Quelldatensatz
uspto-grants-1988_08
Patentnummer
US04767860

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