Реакция #64008

ord-54fa6e31f456499383631172eb6e9555

Уравнение реакции

O=CC=O
glyoxal
CNCCNC
N,N'-dimethylethylenediamine
CN1CCN(C)C(=O)C1
1,4-dimethylpiperazin-2-one
Выход 93.0%

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe solution is heated rapidly
  2. 2
    Температураto reflux
  3. 3
    Температураheating
  4. 4
    Температураmaintained for 5 minutes
  5. 5
    Другоеis then evaporated at 60° C. under water
  6. 6
    workup.DISTILLATIONThe oil is distilled in a short path distillation apparatus

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04767860uspto-grants-1988_08