반응 #77485

ord-4f1d164094b047a693bf9993ac9e2f7b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06706732B1uspto-grants-2004_03