Reaktion #707369

ord-86d15fb1149849e59f5980f320f7c63e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is heated for 2 hours
  2. 2
    Temperaturto reflux
  3. 3
    Temperaturheating
  4. 4
    Temperaturto reflux
  5. 5
    TemperaturThe resulting mixture is cooled
  6. 6
    Sonstigeafter what the organic phase is decanted
  7. 7
    Waschenwashed with water
  8. 8
    Extraktionextracted with a 10% solution of hydrochloric acid
  9. 9
    Extraktionextracted with ether
  10. 10
    Waschenwashed with water
  11. 11
    Trocknendried over magnesium sulfate
  12. 12
    Sonstigeevaporated

Vorschrift

1.95 g of sodium amide are added in small quantities to an ether solution of 9.3 g of 3,4-dichlorophenylacetonitrile. The mixture is heated for 2 hours to reflux, 11.8 g of 2-(4-benzylpiperidino)-1-chloro ethane are added and heating is repeated for another 5 hours to reflux. The resulting mixture is cooled and 200 ml of water are added, after what the organic phase is decanted, washed with water and extracted with a 10% solution of hydrochloric acid. The aqueous phase is then neutralized with soda, extracted with ether, washed with water, dried over magnesium sulfate and evaporated. 13 g of oily product are thus obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04820717uspto-grants-1989_04