Réaction #77485

ord-4f1d164094b047a693bf9993ac9e2f7b

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurethe mixture was heated
  2. 2
    Températureunder reflux for 14 hours
  3. 3
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure
  4. 4
    Autrethe resultant crystal was recrystallized from ethanol

Mode opératoire

A solution of 7-(2,5-difluorophenyl)-4-methyl-5,6,7,8-tetrahydroquinolin-5-one (1.2 g) and aminoguanidine hydrochloride (0.58 g) in ethanol (30 ml) was combined with concentrated hydrochloric acid (1.1 ml) and water (1.1 ml), and the mixture was heated under reflux for 14 hours. The solvent was distilled off under reduced pressure, and the resultant crystal was recrystallized from ethanol to obtain 7-(2,5-difluorophenyl)-5-guanidinoimino-4-methyl-5,6,7,8-tetrahydroquinoline hydrochloride (Compound K) (1.6 g) as a colorless crystal.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06706732B1uspto-grants-2004_03