Reaktion #1330064

ord-63d0d8c3e3d44980a5c951e2d9e98fe4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling
  2. 2
    WaschenThe organic layer was washed with water and saturated aqueous sodium chloride solution
  3. 3
    Sonstigedried
  4. 4
    Einengenconcentrated
  5. 5
    SonstigeThe residue was purified
  6. 6
    Sonstigerecrystallized (THF-IPE)

Vorschrift

Benzoyl chloride (0.14 ml) was added dropwise to pyridine solution (6 ml) of 6-[(4-aminobenzyl)oxy]-2-[(N,N-dimethylamino)methyl]tetralin (300 mg) under ice-cooling, which was stirred at room temperature for 30 minutes. 10% aqueous potassium carbonate solution was added to the reaction mixture, and extraction was conducted using ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride solution, dried, and then concentrated. The residue was purified using alumina column chromatography (development solvent; ethyl acetate), and recrystallized (THF-IPE) to give the titled compound (240 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07115750B1uspto-grants-2006_10