Pyridine → HCID 12944902, Verbindung

HRID 1578266Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1578266
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1Cl)[N:8]([CH2:13][CH3:14])[CH:7]=[C:6]([C:15]([OH:17])=[O:16])[C:5]2=[O:18].[C:19]1([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.N1C=CC=CC=1>C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N:28]1[CH2:29][CH2:30][N:25]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:26][CH2:27]1)[N:8]([CH2:13][CH3:14])[CH:7]=[C:6]([C:15]([OH:17])=[O:16])[C:5]2=[O:18]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 70961-PhenylpiperazineHCID 127338866,7-Dichloro-1-ethyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

Produkt 1

HCID 12944902HCID 12944902, VerbindungAusbeute 54,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

2.15 g of 6,7-dichloro-1-ethyl-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid, 6.5 g of 1-phenylpiperazine and 20 cm3 of pyridine were heated under reflux for 16 hours. The solvent was removed in vacuo and the residue was taken up in 20 cm3 of water. The suspension obtained was stirred and brought to pH 7 by the addition of acetic acid. The solid was filtered off and recrystallised from methyl cellosolve. 1.7 g of 6-chloro-1-ethyl-4-oxo-7-(4-phenylpiperazinyl)-1,4-dihydro-quinoline-3-carboxylic acid, m.p. 234°-235° C., were obtained.

Aufarbeitung

  1. temperatureunder reflux for 16 hours
  2. customThe solvent was removed in vacuo
  3. customThe suspension obtained
  4. filtrationThe solid was filtered off
  5. customrecrystallised from methyl cellosolve

Quellen und Nachweise

ORD-Eintrag
ord-9fb47b30be1144629b35bdc98ebc312d
Quelldatensatz
uspto-grants-1981_09
Patentnummer
US04292317

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