Reaktion #927653
ord-74fea49a9f0c4ff39a1a9519cc837b0f
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturcooling
- 2Sonstigewas carried out to 0° C.
- 3Extraktionextracted with dichloromethane
- 4SonstigeThe organic phase was separated
- 5Waschenwashed with an aqueous sodium bicarbonate solution
- 6Sonstigeevaporated
- 7SonstigeThe product crystallized
- 8FiltrationAfter filtration, 56.9 g (75%) of 2-bromo-5,6,7,8-tetrahydro-3,5,5,8,8-pentamethylnaphthalene
- 9Sonstigea melting-point of 92°-93° C.
- 10Sonstigewere 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.