Reaktion #1552058

ord-08137f861f4e4d6dae76c3d526fbcaa2

Lösungsmittel

Reaktionsbedingungen

Temperatur
3°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONAfter the dropwise addition
  2. 2
    workup.STIRRINGthe mixture was stirred at room temperature for 5 hours
  3. 3
    ExtraktionThe organic layer was extracted with ethyl acetate
  4. 4
    workup.DISTILLATIONthe obtained organic layer was distilled at 40° C. under reduced pressure
  5. 5
    workup.DISTILLATIONfurther distilled at 170° C. under reduced pressure
  6. 6
    Temperaturcooled to room temperature
  7. 7
    Sonstigerecrystallized
  8. 8
    FiltrationThe precipitated crystal was collected by filtration

Vorschrift

Aluminum chloride (6.83 g) was added to 20.0 g of benzene, and the mixture was stirred under cooling at 3° C. Thereto, 40.4 g of cyclohexyl chloride was slowly added dropwise. After the dropwise addition, the mixture was stirred at room temperature for 5 hours and then poured in ice water. The organic layer was extracted with ethyl acetate, and the obtained organic layer was distilled at 40° C. under reduced pressure, further distilled at 170° C. under reduced pressure, then cooled to room temperature, and recrystallized by charging 50 ml of acetone. The precipitated crystal was collected by filtration to obtain 14 g of tricyclohexylbenzene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08999621B2uspto-grants-2015_04