Reaktion #1375337

ord-baaa9391870c42eb8f6ede9532c7d8e9

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONAfter distilling off the hydrochloric acid
  2. 2
    Sonstigethe remaining water was removed by entrainment with benzene
  3. 3
    Sonstigethe raw salt was recrystallized from methanol

Vorschrift

1,2,4,5-Tetrahydro-5-hydroxy-11-methyl-3H-azepino[4,5-b]quinoline dihydrochloride was prepared from 5-(ethoxycarbonyloxy)-1,2,4,5-tetrahydro-11-methyl-3-azepino[4,5-b]quinoline-carboxylic acid ethyl ester by hydrolysis with 2 N hydrochloric acid for 36 hours at the boiling point. After distilling off the hydrochloric acid, the remaining water was removed by entrainment with benzene, and the raw salt was recrystallized from methanol.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US03987047uspto-grants-1976_10