Reaktion #1062292

ord-0e3673a7a9804b678c1d32d4dfba21ed

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was heated
  2. 2
    TemperaturAfter cooling
  3. 3
    Extraktionwas then extracted with isopropyl ether
  4. 4
    WaschenThe organic layer was washed with water
  5. 5
    Trocknendried (anhydrous magnesium sulfate)
  6. 6
    Einengenconcentrated under reduced pressure
  7. 7
    SonstigeThe resulting crude crystals were recrystallized from hexane/isopropyl ether

Vorschrift

To an ethanolic solution (100 ml) of diphenylacetonitrile (28 g) were added DBU (6 ml) and ethyl acrylate (30 ml) and the mixture was heated and stirred at 80° C. for 16 hours. After cooling, 200 ml of 2N-hydrochloric acid was added to the reaction mixture, which was then extracted with isopropyl ether. The organic layer was washed with water, dried (anhydrous magnesium sulfate) and concentrated under reduced pressure. The resulting crude crystals were recrystallized from hexane/isopropyl ether to provide ethyl 4-cyano-4,4-diphenylbutyrate (34 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05607939uspto-grants-1997_03