Reaktion #1183012

ord-caa1868cda204496aeafa1ddeaad0e28

Reaktionsbedingungen

Temperatur
85°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooled to room temperature
  2. 2
    Einengenthis was concentrated
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
  4. 4
    Waschenwashed with aqueous saturated sodium hydrogencarbonate solution and saturated saline
  5. 5
    Trocknenthe organic layer was dried with sodium sulfate
  6. 6
    SonstigeThe solvent was evaporated off
  7. 7
    Sonstigethe 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08138206B2uspto-grants-2012_03