Reaktion #1580066
ord-01d15276a5cc44969c6bb4dae46dbbf6
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThe reaction medium was then reflux-heated for 4 hours
- 2Temperaturthe reaction medium was again reflux-heated for 2 days
- 3EinengenAfter concentration
- 4Sonstigeby evaporation of the solvent
- 5workup.DISSOLUTIONthe residue was dissolved in 20 ml of 10% aqueous NaOH
- 6FiltrationAfter filtration
- 7Extraktionthe aqueous phase was extracted with ether
Vorschrift
6.6×10-2 mol of sodium azide and 6.6×10-2 mol of acetic acid were added to a solution of 5×10-2 mol of 4-benzyloxy benzonitrile (VIII) in 20 ml butanol. The reaction medium was then reflux-heated for 4 hours. 1 g sodium azide, 2 g acetic acid and 10 ml butanol were added and the reaction medium was again reflux-heated for 2 days. After concentration by evaporation of the solvent, the residue was dissolved in 20 ml of 10% aqueous NaOH. After filtration, the aqueous phase was extracted with ether. The alkaline solution was acidified with 2N HCl to obtain the expected compound, which was isolated with an 85% yield (M.P.=228° C.).