Reaktion #49675
ord-978206fb8dd144ab90f2e261895a7ce5
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas heated
- 2Temperaturunder reflux for 7 hours
- 3SonstigeThe mixture was partitioned between dichloromethane (30 ml) and 10% aqueous sodium carbonate (30 ml)
- 4Sonstigethe layers separated
- 5Extraktionthe aqueous layer extracted with dichloromethane (2×30 ml)
- 6TrocknenThe combined dichloromethane extracts were dried (MgSO4)
- 7Einengenconcentrated in vacuo
- 8Sonstigeto give a colourless solid which
- 9Sonstigewas 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.