Reaktion #1842129

ord-65aad95bbdfa434dbb873b76d27c9e16

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe organic layer and the aqueous layer were separated
  2. 2
    Einengenthe organic layer was then concentrated under reduced pressure
  3. 3
    SonstigeThe resulting residue was triturated with ethyl acetate:n-hexane (1:4, 200 mL)
  4. 4
    Filtrationfiltered
  5. 5
    Einengenthe filtrate was concentrated under reduced pressure
  6. 6
    SonstigeThe residue was purified by silica gel column chromatography

Vorschrift

Triphenylphosphine (7.83 g, 29.8 mmol) and carbon tetrabromide (12.4 g, 37.3 mmol) were added to a solution of 2-(2-bromophenyl)ethanol (5.00 g, 24.9 mmol) in dichloromethane (123 mL). The mixture was stirred at room temperature for 15 hours, and a saturated aqueous sodium carbonate solution was then added. The organic layer and the aqueous layer were separated, and the organic layer was then concentrated under reduced pressure. The resulting residue was triturated with ethyl acetate:n-hexane (1:4, 200 mL) and then filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 1-bromo-2-(2-bromoethyl)benzene as a colorless oil (6.23 g, 95%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09169254B2uspto-grants-2015_10