Chlorocyclohexane → Tricyclohexylbenzene

HRID 590894

Reaktionsgleichung

[Cl-].[Al+3].[Cl-].[Cl-].[CH:5]1(Cl)[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1>C1C=CC=CC=1>[CH:5]1([C:5]2[C:6]([CH:5]3[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]3)=[C:7]([CH:5]3[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]3)[CH:8]=[CH:9][CH:10]=2)[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1

Komponenten

Reaktionsbedingungen

Temperatur: 3 °C

Versuchsvorschrift

First, 6.83 g of aluminum chloride was added to 20.0 g of benzene, and agitated while cooling at 3° C. Then, 40.4 g of cyclohexyl chloride was slowly dropped thereinto. After the completion of the dropping, the mixture was agitated at room temperature for five hours and poured into ice water. The organic phase was extracted with ethyl acetate, and the obtained organic phase was subjected to vacuum distillation at 40° C. Further, vacuum distillation was performed at 170° C., and the product was cooled to room temperature. Thereafter, 50 ml of acetone was placed thereinto, and recrystallization was carried out. The resultant crystal was collected by filtration. Thus, 14 g of tricyclohexylbenzene was obtained.

Aufarbeitung

stirringAfter the completion of the dropping, the mixture was agitated at room temperature for five hours
extractionThe organic phase was extracted with ethyl acetate
distillationthe obtained organic phase was subjected to vacuum distillation at 40° C
distillationFurther, vacuum distillation
customwas performed at 170° C.
temperaturethe product was cooled to room temperature
customrecrystallization
filtrationThe resultant crystal was collected by filtration

Quellen und Nachweise

ORD-Eintrag: ord-f89bd6f5c9d24abb8d5381c2aa50dcee
Quelldatensatz: uspto-grants-2016_01
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09235116B2

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