Reaktion #1114530

ord-a814e97254c744a39b40b1903e1b537c

Lösungsmittel

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    workup.ADDITIONafter the dropwise addition
  2. 2
    workup.STIRRINGthe reaction solution 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 off under reduced pressure at 40° C.
  5. 5
    workup.DISTILLATIONfurther distilled off under reduced pressure at 170° C.
  6. 6
    Temperaturcooled to room temperature
  7. 7
    Sonstigerecrystallized
  8. 8
    FiltrationThe precipitated crystals were collected by filtration

Vorschrift

6.83 g of aluminum chloride was added to 20.0 g of benzene, and the mixture was stirred under cooling at 3° C. Subsequently, 40.4 g of cyclohexyl chloride was slowly added dropwise and after the dropwise addition, the reaction solution 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 off under reduced pressure at 40° C., further distilled off under reduced pressure at 170° C., then cooled to room temperature and recrystallized by charging 50 ml of acetone thereinto. The precipitated crystals were collected by filtration to obtain 14 g of tricyclohexylbenzene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08735048B2uspto-grants-2014_05