Reaktion #2178361

ord-4f07b6612afe40f8963917f8129a0926

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto quench
  2. 2
    Sonstigethe reaction
  3. 3
    Extraktionthe reaction mixture was extracted with ethyl acetate
  4. 4
    WaschenThe extract was washed with saturated brine
  5. 5
    Trocknendried over magnesium sulfate
  6. 6
    Einengenconcentrated under reduced pressure
  7. 7
    SonstigeThe residue was purified by silica gel column chromatography (6% ethyl acetate/hexane)

Vorschrift

To a mixture of 5-methoxy-3-methyl-1-benzofuran (2.00 g) synthesized above, 2-ethylbutanoyl chloride (1.85 mL) and nitromethane (30 mL) was added aluminum chloride (3.28 g), and the mixture was stirred at room temperature for 1.5 hr. Water was added to quench the reaction, and the reaction mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (6% ethyl acetate/hexane) to give the title object compound (3.12 g, 97%) as a pale-yellow oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08436043B2uspto-grants-2013_05