Reaktion #5308

ord-ac03c135aa2e493cb63eaf76ba6c32fa

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe suspension was refluxed for 20 h
  2. 2
    ExtraktionThe resulting emulsion was extracted with ER (2×50 ml)
  3. 3
    Extraktionthe dried extract
  4. 4
    Sonstigewas evaporated
  5. 5
    Sonstigeto leave a yellow oil
  6. 6
    SonstigeThe oil was purified on a column of silica (Merck 9385, 600 ml) [A]

Vorschrift

NaH (46% dispersion in oil; 1.36 g) was added portionwise to a solution of 2-methoxybenzenebutanol (5.0 g) and 1,6-dibromohexane (13.8 g) in THF (50 ml). The suspension was refluxed for 20 h and was treated cautiously with H2O (20 ml). The resulting emulsion was extracted with ER (2×50 ml) and the dried extract was evaporated to leave a yellow oil. The oil was purified on a column of silica (Merck 9385, 600 ml) [A] to give the title compound as a colourless oil (5.6 g). T.l.c. [B] Rf 0.2.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05243076uspto-grants-1993_09