Hydrochloric Acid → HCID 178428136, Verbindung

HRID 49207Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 49207
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH:9]1[CH2:18][C:17]2[N:16]=[CH:15][CH:14]=[C:13]([CH3:19])[C:12]=2[C:11](=O)[CH2:10]1.[C:21]([NH:24][NH2:25])([NH2:23])=[NH:22].[ClH:26].Cl.O>C(O)C>[ClH:26].[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH:9]1[CH2:18][C:17]2[N:16]=[CH:15][CH:14]=[C:13]([CH3:19])[C:12]=2[C:11](=[N:25][NH:24][C:21]([NH2:23])=[NH:22])[CH2:10]1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 110869317-(2,5-Difluorophenyl)-4-methyl-5,6,7,8-tetrahydroquinolin-5-oneHCID 178418668HCID 178418668, Verbindung

Produkt 1

HCID 178428136HCID 178428136, VerbindungAusbeute 99,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 14 hours
  3. distillationThe solvent was distilled off under reduced pressure
  4. customthe resultant crystal was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-4f1d164094b047a693bf9993ac9e2f7b
Quelldatensatz
uspto-grants-2004_03
Patentnummer
US06706732B1

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