Reaktion #1074523

ord-b5dfeabbdc19488cbc2b002fe0a6b492

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated under reduced pressure
  2. 2
    Sonstigethe crude oil obtained
  3. 3
    Filtrationwas filtered through a pad of silica gel
  4. 4
    WaschenElution with petroleum ether (b.p. 40-60° C.)
  5. 5
    Sonstigegave a colourless fraction
  6. 6
    WaschenThe silica gel was then eluted with acetone

Vorschrift

1,12-Dodecanediol (50 g, 0.25 mol) in hydrogen bromide 48% (220 ml) was continuously extracted with petroleum ether (b.p. 80-100° C.) (300 ml) for 18 hours. The solvent was evaporated under reduced pressure and the crude oil obtained was filtered through a pad of silica gel. Elution with petroleum ether (b.p. 40-60° C.) gave a colourless fraction containing 1,12-dibromododecane. The silica gel was then eluted with acetone to give the title compound as a pale yellow oil after evaporation of the solvent. The title compound crystallised upon cooling and was recrystallised from petroleum ether (b.p. 40-60° C.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06630128B1uspto-grants-2003_10