Reaktion #215568

ord-4e19cbcd52f644bc8a211320478bf3bc

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe solution was cooled to 0° to 5° C.
  2. 2
    workup.STIRRINGThe mixture was stirred for 30 minutes
  3. 3
    SonstigeThe precipitate was separated by filtration
  4. 4
    EinengenThe filtrate was concentrated under reduced pressure
  5. 5
    Sonstigeto afford a yellow oily product
  6. 6
    Sonstigethe precipitated white powder was recrystallized from ethanol

Vorschrift

2,3-Dicyano-5-chloro-6-ethylpyrazine (1.92 g; 0.01 mole) was dissolved in 30 ml of acetone. The solution was cooled to 0° to 5° C., and with stirring, 2.02 g (0.02 mole) of di-n-propylamine was added dropwise. The mixture was stirred for 30 minutes. The precipitate was separated by filtration. The filtrate was concentrated under reduced pressure to afford a yellow oily product. Water (20 ml) was added to the oily product, and the precipitated white powder was recrystallized from ethanol to afford 1.28 g (yield 50%) of 2,3-dicyano-5-di-n-propylamino-6-ethylpyrazine.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04259489uspto-grants-1981_03