Reaktion #1013623

ord-07539820e33d4892b166061072dcd109

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 off under reduced pressure at 40° C
  5. 5
    workup.DISTILLATIONAfter further distillation off under reduced pressure at 170° C.
  6. 6
    Temperaturthe product was cooled to room temperature
  7. 7
    workup.ADDITIONcharged into 50 ml of acetone
  8. 8
    Sonstigerecrystallized
  9. 9
    SonstigeThe crystal precipitated
  10. 10
    Filtrationwas collected by filtration

Vorschrift

6.83 g of aluminum chloride was added to 20.0 g of benzene, followed by cooling/stirring at 3° C., and 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 poured into ice water. The organic layer was extracted with ethyl acetate, and the obtained organic layer was distilled off under reduced pressure at 40° C. After further distillation off under reduced pressure at 170° C., the product was cooled to room temperature, charged into 50 ml of acetone and thereby recrystallized. The crystal precipitated was collected by filtration to obtain 14 g of tricyclohexylbenzene.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09285679B2uspto-grants-2016_03