Reaktion #63798

ord-0a808d8832164fd696ba306bfcf7bb18

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxing
  2. 2
    Temperaturare maintained for 3 hours
  3. 3
    Temperaturthe reaction mixture is then cooled
  4. 4
    Sonstigethe ethanol evaporated off under reduced pressure
  5. 5
    workup.STIRRINGThe evaporation residue is stirred in 700 ml of water at 70° C. for 3 hours
  6. 6
    Filtrationthe insoluble material is then filtered off
  7. 7
    Waschenwashed with 50 ml of ethanol
  8. 8
    Trocknenether and dried

Vorschrift

59.5 g (0.2 mole) of 1-bromo-2-(4-nitrophenyl)-2-ethanone, 21.6 g (0.2 mole) of 2-amino-5-methylpyridine and 34 g of sodium bicarbonate are reacted in 200 ml of 95% strength ethanol. Stirring and refluxing are maintained for 3 hours, and the reaction mixture is then cooled and the ethanol evaporated off under reduced pressure. The evaporation residue is stirred in 700 ml of water at 70° C. for 3 hours, and the insoluble material is then filtered off, washed with 50 ml of ethanol and then ether and dried. M.p. 237°-239° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04767755uspto-grants-1988_08