Reaktion #927653

ord-74fea49a9f0c4ff39a1a9519cc837b0f

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling
  2. 2
    Sonstigewas carried out to 0° C.
  3. 3
    Extraktionextracted with dichloromethane
  4. 4
    SonstigeThe organic phase was separated
  5. 5
    Waschenwashed with an aqueous sodium bicarbonate solution
  6. 6
    Sonstigeevaporated
  7. 7
    SonstigeThe product crystallized
  8. 8
    FiltrationAfter filtration, 56.9 g (75%) of 2-bromo-5,6,7,8-tetrahydro-3,5,5,8,8-pentamethylnaphthalene
  9. 9
    Sonstigea melting-point of 92°-93° C.
  10. 10
    Sonstigewere recovered

Vorschrift

30 ml of 2-bromotoluene and 14 g (0.11 mol) of AlCl3 were introduced into a three-necked flask, cooling was carried out to 0° C. and a solution of 50 g (0.27 mol) of 2,5-dichloro-2,5-dimethylhexane in 100 ml of 2-bromotoluene was added dropwise, and the reaction mixture was permitted to heat to room temperature. The reaction mixture was poured into water and extracted with dichloromethane. The organic phase was separated by settling, washed with an aqueous sodium bicarbonate solution and evaporated. The product crystallized on stirring in methanol. After filtration, 56.9 g (75%) of 2-bromo-5,6,7,8-tetrahydro-3,5,5,8,8-pentamethylnaphthalene, with a melting-point of 92°-93° C., were recovered.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06368608B1uspto-grants-2002_04