Reaktion #54279

ord-551580bfd33349668c8de1563891ed34

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONTo the resulting solution are added 0.5 g
  2. 2
    SonstigeAfter the absorption of hydrogen
  3. 3
    Temperaturthe mixture is cooled
  4. 4
    FiltrationThen the catalyst is filtered off
  5. 5
    Einengenthe filtrate is concentrated to dryness
  6. 6
    SonstigeUpon recrystallization of the crude crystalline residue from isopropyl alcohol, 12.5 g

Vorschrift

18 g. of 1-(3,4-methylenedioxyphenyl)-2-aminoethanol hydrochloride are dissolved in 300 ml. of ethanol and 50 ml. of 80% aqueous solution of acetaldehyde. To the resulting solution are added 0.5 g. of extended Raney nickel and the mixture is heated at 70° C. in an atmosphere of hydrogen in a 1 liter-autoclave. After the absorption of hydrogen is complete, the mixture is cooled. Then the catalyst is filtered off and the filtrate is concentrated to dryness. Upon recrystallization of the crude crystalline residue from isopropyl alcohol, 12.5 g. of 1-(3,4-methylenedioxyphenyl)-2-ethylaminoethanol hydrochloride are obtained as white needles.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04147799uspto-grants-1979_04