Reaktion #673829

ord-637c68d4018245a8a8e4664c6851ea9f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with ice-water (1×10 mL), 10% HCl (1×10 mL) and brine (1×10 mL)
  2. 2
    Trocknendried (MgSO4)
  3. 3
    Einengenconcentrated
  4. 4
    Sonstigeto afford a brown oil
  5. 5
    workup.DISTILLATIONThe crude was then distilled
  6. 6
    workup.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:

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06936636B2uspto-grants-2005_08