Reaktion #64008

Reaktionsgleichung

glyoxal

N,N'-dimethylethylenediamine

→

1,4-dimethylpiperazin-2-one

Ausbeute 93.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe solution is heated rapidly
2. 2
   Temperaturto reflux
3. 3
   Temperaturheating
4. 4
   Temperaturmaintained for 5 minutes
5. 5
   Sonstigeis then evaporated at 60° C. under water
6. 6
   workup.DISTILLATIONThe oil is distilled in a short path distillation apparatus

Vorschrift

To 10 g (69.0 mmoles) of 40 percent glyoxal and 200 ml of distilled water is rapidly added 6.1 g (69.0 mmoles) of N,N'-dimethylethylenediamine. 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 8.2 g (93 percent yield) of 1,4-dimethylpiperazin-2-one in the form of a yellow oil. Purity is greater than 99 percent by capillary gas chromatograph.

Quelle