Reaktion #359441

ord-c9a630da5e8346fa98bc5ac0062931cb

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturunder reflux on a steam-bath for 1.5 h
  2. 2
    Temperaturto cool
  3. 3
    workup.DISTILLATIONbefore being distilled under reduced pressure
  4. 4
    Sonstigeto remove volatiles
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in 60-80 petroleum-ether (200 ml)
  6. 6
    workup.DISTILLATIONthe solution was distilled under reduced pressure
  7. 7
    Sonstigeto remove any remaining traces of volatiles

Vorschrift

2-(2,4-Di-t-pentylphenoxy)ethanoic acid (12.0 g, 0.041 mol) (CAS Registry Number 13402-96-5) and thionyl chloride (60 ml) were heated under reflux on a steam-bath for 1.5 h. The resulting yellow solution was allowed to cool before being distilled under reduced pressure to remove volatiles. The residue was dissolved in 60-80 petroleum-ether (200 ml) and the solution was distilled under reduced pressure to remove any remaining traces of volatiles, leaving 2-(2,4-di-t-pentyl-phenoxy)ethanoyl chloride as a red oil which was used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07455959B2uspto-grants-2008_11