Reaktion #353853

ord-761b847cf8e74abd96bbc3c1bb21f911

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONadded portionwise to the solution
  2. 2
    Extraktionthe mixture was extracted with hexane
  3. 3
    WaschenThe organic layer was washed each twice with water, aqueous sodium hydrogen carbonate
  4. 4
    Trocknenwith water, dried over MgSO4
  5. 5
    Sonstigethe solvent was removed by evaporation
  6. 6
    workup.DISTILLATIONThe residue was distilled

Vorschrift

2,5-Dichloro-2,5-dimethylhexane (67.5 g, 0.369 mol) was dissolved in dry toluene (200 ml), and then AlCl3 (4.05 g, 30.4 mmol) was crushed up and added portionwise to the solution. After being left for 2 hours, the reaction mixture was poured into ice/5% HCl and the mixture was extracted with hexane. The organic layer was washed each twice with water, aqueous sodium hydrogen carbonate, and then with water, dried over MgSO4, and the solvent was removed by evaporation. The residue was distilled to give 5,6,7,8-tetrahydro-2,5,5,8,8-pentamethylnaphthalene (70.42 g, yield: 90%). bp 100° C. (solidified at room temperature).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05652232uspto-grants-1997_07