Reaktion #1816154

ord-62485f68e7e2466fb607327cdf1461e7

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe phases were separated
  2. 2
    ExtraktionThe aqueous phase was extracted 4 times with 250 ml of toluene each time
  3. 3
    Waschenthe combined organic phases were washed with saturated aqueous NaHCO3 solution and NaCl solution
  4. 4
    Trocknendried over MgSO4
  5. 5
    SonstigeThe solvent was removed in vacuo
  6. 6
    workup.DISTILLATIONthe residue was distilled (78° C./0.2 mmHg)

Vorschrift

101.7 g (0.48 mol) of 2-(2-methyl-benzyl)-butyryl chloride (e2) were added dropwise to 191 g (1.43 mol) of AlCl3 in 600 ml of toluene, and the mixture was heated at 80° C. for about 3.5 hours. The reaction mixture was poured onto 1 l of ice/concentrated HCl, and the phases were separated. The aqueous phase was extracted 4 times with 250 ml of toluene each time, and the combined organic phases were washed with saturated aqueous NaHCO3 solution and NaCl solution and dried over MgSO4. The solvent was removed in vacuo and the residue was distilled (78° C./0.2 mmHg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05329033uspto-grants-1994_07