Reaktion #49675

ord-978206fb8dd144ab90f2e261895a7ce5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturunder reflux for 7 hours
  3. 3
    SonstigeThe mixture was partitioned between dichloromethane (30 ml) and 10% aqueous sodium carbonate (30 ml)
  4. 4
    Sonstigethe layers separated
  5. 5
    Extraktionthe aqueous layer extracted with dichloromethane (2×30 ml)
  6. 6
    TrocknenThe combined dichloromethane extracts were dried (MgSO4)
  7. 7
    Einengenconcentrated in vacuo
  8. 8
    Sonstigeto give a colourless solid which
  9. 9
    Sonstigewas recrystallised from aqueous ethanol

Vorschrift

A mixture containing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)piperidine (0.3 g), phenethyl bromide (0.2 g), anhydrous potassium carbonate (0.3 g) and acetonitrile (10 ml) was heated under reflux for 7 hours. The mixture was partitioned between dichloromethane (30 ml) and 10% aqueous sodium carbonate (30 ml), the layers separated, and the aqueous layer extracted with dichloromethane (2×30 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give a colourless solid which was recrystallised from aqueous ethanol to give the title compound, yield, 0.17 g, m.p. 175°-1780° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05422358uspto-grants-1995_06