Reaktion #1183012
ord-caa1868cda204496aeafa1ddeaad0e28
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
85°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturAfter cooled to room temperature
- 2Einengenthis was concentrated
- 3workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
- 4Waschenwashed with aqueous saturated sodium hydrogencarbonate solution and saturated saline
- 5Trocknenthe organic layer was dried with sodium sulfate
- 6SonstigeThe solvent was evaporated off
- 7Sonstigethe residue was purified through silica gel column chromatography (eluate: ethyl acetate/hexane=50/50 to chloroform/methanol=10/1)
Vorschrift
1-[(3-chloropropyl)oxy]-4-iodobenzene (10 g, 33.7 mmol) and piperidine (2.87 g, 67.4 mmol) were mixed, and stirred at 85° C. for 4 hours. After cooled to room temperature, this was concentrated, and the residue was dissolved in ethyl acetate, washed with aqueous saturated sodium hydrogencarbonate solution and saturated saline, and the organic layer was dried with sodium sulfate. The solvent was evaporated off, and the residue was purified through silica gel column chromatography (eluate: ethyl acetate/hexane=50/50 to chloroform/methanol=10/1) to obtain the entitled compound (8.39 g, 72%) as a brown solid.