Reaktion #485485

ord-39072a6ec0c646aa996354032aa94953

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwhile cooling with ice
  2. 2
    workup.ADDITIONwas added dropwise
  3. 3
    Extraktionextracted with ethyl acetate
  4. 4
    Trocknendried over sodium sulphate
  5. 5
    Sonstigeevaporated
  6. 6
    workup.DISTILLATIONThe crude product was distilled in a high vacuum

Vorschrift

83 ml of hexylbenzene were treated with 1.8 g of aluminium chloride while cooling with ice. After brief stirring a solution of 40 g of 2,5-dichloro-2,5-dimethyl-hexane in 300 ml of carbon disulphide was added dropwise and the mixture was stirred at 0° C. for a further 2 hours. The reaction mixture was poured into ice/6N hydrochloric acid, extracted with ethyl acetate, dried over sodium sulphate and evaporated. The crude product was distilled in a high vacuum. There were obtained 25.5 g of 1,1,4,4-tetramethyl-6-hexyl-1,2,3,4-tetrahydro-naphthalene as a colourless oil, boiling point 141-152° C./0.8 mm.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06610877B1uspto-grants-2003_08