Methanol → 1,4-Di(n-butyl)piperazin-2-one

HRID 35732

Reaktionsgleichung

Reaktionsgleichung von HRID 35732
[CH:1]([CH:3]=O)=[O:2].CO.[CH2:7]([NH:11][CH2:12][CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH2:8][CH2:9][CH3:10]>O1CCOCC1>[CH2:15]([N:14]1[CH2:13][CH2:12][N:11]([CH2:7][CH2:8][CH2:9][CH3:10])[CH2:3][C:1]1=[O:2])[CH2:16][CH2:17][CH3:18]

Komponenten

5

Edukt 3

HCID 887MethanolHCID 7860GlyoxalHCID 77629N,N'-Dibutylethylenediamine

Produkt 1

HCID 142506501,4-Di(n-butyl)piperazin-2-oneAusbeute 30,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To 10 g (69.0 mmoles) of 40 percent glyoxal and 200 ml of methanol is rapidly added 11.9 g (69.0 mmoles) of N,N'-di(n-butyl)ethylenediamine. The solution is rapidly brought to reflux and heating is maintained for 5 minutes. The dark brown solution is then allowed to cool to room temperature at which time fine white crystals precipitate from the brown oil. The oil is diluted with 100 ml of 1,4-dioxane and the solid is removed by filtration. The dioxane solution is concentrated under aspirator vacuum and distilled in a short path distillation apparatus to give 4.5 g of 1,4-di(n-butyl)piperazin-2-one in the form of a brown oil (31 percent yield).

Aufarbeitung

  1. temperatureto reflux
  2. temperatureheating
  3. temperatureis maintained for 5 minutes
  4. customthe solid is removed by filtration
  5. concentrationThe dioxane solution is concentrated under aspirator vacuum
  6. distillationdistilled in a short path distillation apparatus

Quellen und Nachweise

ORD-Eintrag
ord-94d3d49cf1044e7883ab64fe7800a8d7
Quelldatensatz
uspto-grants-1988_08
Patentnummer
US04767860

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