Reaktion #484018

ord-31df67c1863d4d3e9bbd99d118b2faf5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture was heated
  2. 2
    Temperaturat reflux temperature for 16 hours
  3. 3
    workup.ADDITIONpoured into ice
  4. 4
    ExtraktionThe whole was extracted with diethyl ether
  5. 5
    WaschenThe organic layer was washed with brine
  6. 6
    Trocknendried over MgSO4
  7. 7
    Einengenconcentrated in vacuo

Vorschrift

To a stirred solution of 2-ethylphenol (13 g, 106.4 mmol) in carbon disulfide (30 ml) was added aluminum chloride (30 g, 225 mmol) portionwise at 0° C. Then, acetyl chloride (8.4 ml, 118.1 mmol) was added, and the mixture was heated at reflux temperature for 16 hours. The reaction mixture was cooled down to room temperature, and poured into ice. The whole was extracted with diethyl ether. The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was recystallized with hexane-toluene to give title compound (9.24 g, 53% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06608095B2uspto-grants-2003_08