Реакция #1195628

ord-3a6534d12689498b86c2dbd29d1ec24c

Реагенты

Нет

Растворители

Условия реакции

Температура
20°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.STIRRINGthe mixture was stirred at 0° C. for 2 hours
  2. 2
    ТемператураThe solution was then cooled to -20° C
  3. 3
    ДругоеThe product precipitated out
  4. 4
    ФильтрацияAfter filtration
  5. 5
    Другоеdrying

Методика

Under argon, 6 g (60.5 mmol) of 2-amino-2-cyanoacetamide was initially charged in 67 g of methanol. 1.67 g (9.3 mmol) of sodium methoxide solution (30%) was added and the mixture was stirred at 20° C. for 2 hours. At 0° C., 11.55 g (64.1 mmol) of methylglyoxal solution (40%) was added and the mixture was stirred at 0° C. for 2 hours. The solution was then cooled to -20° C. The product precipitated out. After filtration and drying, 3.56 g of the title product was obtained. The yield was 39 percent. The melting point of the title product was 170° C. to 172° C. Other data concerning the title product was:

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06066736uspto-grants-2000_05