Reaktion #49673

ord-2c0f66410bbd4d81851ffca9017a268d

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturunder reflux for 16 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
    Trocknendried (MgSO4)
  7. 7
    Einengenconcentrated in vacuo
  8. 8
    Sonstigeto give a solid which
  9. 9
    Sonstigewas recrystallised from ethanol

Vorschrift

A mixture containing 3-(R,S)-(1-carbamoyl-1,1-diphenylmethyl)piperidine (0.26 g), 1-bromo-3-(4-methoxyphenyl)propane (0.23 g), anhydrous potassium carbonate (0.3 g) and acetonitrile (10 ml) was heated under reflux for 16 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 dichloromethane extracts were combined, dried (MgSO4) and concentrated in vacuo to give a solid which was recrystallised from ethanol to give the title compound, yield 0.19 g, m.p. 180°-182° C.

Quelle

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