Reaktion #2342
ord-b7642883f03a44b1a3f521f0f19b94b6
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.STIRRINGstirring
- 2workup.WAITcontinued for 20 hours
- 3Extraktionthe mixture extracted three times with ethyl acetate
- 4WaschenThe combined extracts were washed with water and brine
- 5Trocknendried (MgSO4)
- 6Sonstigeevaporated
- 7SonstigeThe residue was triturated with hexane
- 8Filtrationfiltered
Vorschrift
Sodium hydride (60% dispersion in mineral oil, 0.4 g) was added to a stirred suspension of 4-[4-(4-pyridyl)piperazin-1-yl]phenol (2.55 g) in DMF (25 ml) and the mixture stirred for 20 minutes at room temperature. Allyl chloride (0.756 g) was added dropwise and stirring continued for 20 hours. Ice-water (75 ml) was added and the mixture extracted three times with ethyl acetate. The combined extracts were washed with water and brine, dried (MgSO4) and evaporated. The residue was triturated with hexane and filtered to give 4-[4-(4-pyridyl)piperazin-1-yl]phenol allyl ether (2.5 g) as a solid;