Reaktion #93449

ord-b560ce693e69461abe495ea6b34886be

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationFiltration of the mixture and concentration of the filtrate
  2. 2
    Sonstigegave a white semi-crystalline residue which
  3. 3
    Sonstigeafter recrystallization from 100 ml of hexane

Vorschrift

2.20 g of 4-(trans-4-pentylcyclohexyl)-4'-[2-(trans-4-pentylcyclohexyl)vinyl]biphenyl were suspended in toluene/ethanol (3:2) in a sulphonation flask, treated with 200 mg of palladium/carbon (10%) and hydrogenated at normal pressure and 50° C. until the hydrogen uptake came to a standstill. Filtration of the mixture and concentration of the filtrate gave a white semi-crystalline residue which, after recrystallization from 100 ml of hexane, yielded 1.55 g of 4-(trans-4-pentylcyclohexyl)-4'-[2-(trans-4-pentylcyclohexyl)ethyl]biphenyl as colourless needles; transition (presumably S-S) 219.5° C., transition S-N 243.2° C., cl.p. (N-I) 256.1° C. This substance was found to be very strongly super-coolable; upon cooling to room temperature it still did not crystallize. Rf-value (hexane): 0.32.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04613208uspto-grants-1986_09