Reaktion #2348095

ord-cceab7d6b01d41648ed8e8bd2d9a833e

Reaktionsgleichung

[H][H]
hydrogen
CCCC1CCC(C2CCC(C=Cc3c(C)cc(OCC)c(F)c3F)CC2)CC1
compound 1-3-3-9
CCCC1CCC(C2CCC(C=Cc3c(C)cc(OCC)c(F)c3F)CC2)CC1
1-(2,3-difluoro-4-ethoxy-6-methylphenyl)-2-(4-(4-propylcyclohexyl)cyclohexyl)ethene
CCCC1CCC(C2CCC(CCc3c(C)cc(OCC)c(F)c3F)CC2)CC1
1-(2,3-difluoro-4-ethoxy-6-methylphenyl)-2-(4-(4-propylcyclohexyl)cyclohexyl)ethane
Ausbeute 80.7%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewas not absorbed
  2. 2
    SonstigePd/C was removed
  3. 3
    workup.DISTILLATIONthe solvent was distilled off
  4. 4
    SonstigeThe residue was purified by silica gel column chromatography and recrystallization

Vorschrift

0.31 g of Pd/C was added to 6.20 g of the compound 1-3-3-9 having been dissolved in 50 mL of toluene and 50 mL of Solmix, and under a hydrogen atmosphere, the mixture was stirred at room temperature until hydrogen was not absorbed. Pd/C was removed, and the solvent was distilled off. The residue was purified by silica gel column chromatography and recrystallization to obtain 5.03 g of 1-(2,3-difluoro-4-ethoxy-6-methylphenyl)-2-(4-(4-propylcyclohexyl)cyclohexyl)ethane (Compound 1-3-3-1) as colorless crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07846513B2uspto-grants-2010_12