Reaktion #1253704

ord-146cfd21403046fda72e7ae17a8fbb01

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was heated
  2. 2
    Temperaturunder reflux for 90 minutes
  3. 3
    ExtraktionThen, this was extracted with ethyl acetate
  4. 4
    WaschenThe organic layer was washed with water
  5. 5
    Trocknena saturated aqueous sodium chloride solution, then dried
  6. 6
    Einengenconcentrated
  7. 7
    SonstigeThe residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/1)

Vorschrift

6-Acetylamino-2-(N,N-dimethylamino)methyltetralin hydrochloride (0.879 g; obtained in Reference Example 31) was added to 2 N hydrochloric acid. The reaction mixture was heated under reflux for 90 minutes, and then an aqueous solution of 1 N sodium hydroxide was added thereto to thereby make the resulting mixture have pH of 9. Then, this was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous sodium chloride solution, then dried, and concentrated. The residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/1) to obtain the entitled compound (0.231 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06613805B2uspto-grants-2003_09