Reaktion #673829
ord-637c68d4018245a8a8e4664c6851ea9f
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Waschenwashed with ice-water (1×10 mL), 10% HCl (1×10 mL) and brine (1×10 mL)
- 2Trocknendried (MgSO4)
- 3Einengenconcentrated
- 4Sonstigeto afford a brown oil
- 5workup.DISTILLATIONThe crude was then distilled
- 6workup.DISTILLATIONCoughler distillation
Vorschrift
Aluminum chloride (700 mg, 5.25 mmol) was added slowly to a solution of 2,5-dichloro-2,5-dimethylhexane (11 g, 60 mmol) in bromobenzene (90 mL) at 0° C. After stirred for 20 min, the mixture was diluted with 100 mL of ether:hexane (1:1), washed with ice-water (1×10 mL), 10% HCl (1×10 mL) and brine (1×10 mL), dried (MgSO4) and concentrated to afford a brown oil. The crude was then distilled using Coughler distillation to yield the title compound (13.2 g, 83% yield) as a white solid: