Reaktion #1787786

ord-e3f6d92754f840a2b30abb60304eb2a4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed for 13.5 hours
  2. 2
    SonstigeUnder reduced pressure, the solvent was evaporated
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in water
  4. 4
    WaschenThe solution was washed with ethyl acetate
  5. 5
    SonstigeUnder reduced pressure, the solvent was evaporated
  6. 6
    Sonstigethe residue was recrystallized from ethanol

Vorschrift

A mixture of 7-(2-chlorophenyl)-2,4-dimethyl-5,6,7,8-tetrahydroquinolin-5-one (0.20 g), aminoguanidine hydrochloride (0.081 g), concentrated hydrochloric acid (0.1 ml), water (0.1 ml) and ethanol (20 ml) was refluxed for 13.5 hours. Under reduced pressure, the solvent was evaporated, and the residue was dissolved in water. The solution was washed with ethyl acetate. Under reduced pressure, the solvent was evaporated, and the residue was recrystallized from ethanol to give 7-(2-chlorophenyl)-5-guanidinoimino-2,4-dimethyl-5,6,7,8-tetrahydroquinoline hydrochloride (Compound 86) (0.11 g) as colorless crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06350749B1uspto-grants-2002_02