1-Methylpiperazine → HCID 12733914, Verbindung

HRID 544222Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 544222
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([Cl:14])=[C:10](Cl)[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([OH:18])=[O:17])=[CH:4]1)[CH3:2].[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>O>[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([Cl:14])=[C:10]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([OH:18])=[O:17])=[CH:4]1)[CH3:2]

Komponenten

4

Edukt 2

HCID 531671-MethylpiperazineHCID 127338866,7-Dichloro-1-ethyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

Produkt 1

HCID 12733914HCID 12733914, VerbindungAusbeute 30 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 1-ethyl-6,7-dichloro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid 2.86 g (0.01 mole), N-methylpiperazine 10 g (0.1 mole) and 15 ml water was heated in a sealed tube at 125°-130° C. (inner temperature) for 19 hours. After cooling, the reaction mixture was evaporated under vacuum and acidified with acetic acid. Insoluble matters were filtered off and the filtrate was neutralized with an aqueous solutiong of NaOH to pH 7, extracted with CHCl3, dried with anhydrous Na2SO4, and the solvent was distilled off. The residue was recrystallized from a mixed solvent of CHCl3 and benzene to give 1.05 g (30%) of 1-ethyl-6-chloro-7-(4-methyl-1-piperazinyl)-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid. Colorless needles.

Aufarbeitung

  1. temperaturewas heated in a sealed tube at 125°-130° C. (inner temperature) for 19 hours
  2. temperatureAfter cooling
  3. customthe reaction mixture was evaporated under vacuum
  4. filtrationInsoluble matters were filtered off
  5. extractionextracted with CHCl3
  6. dry with materialdried with anhydrous Na2SO4
  7. distillationthe solvent was distilled off
  8. customThe residue was recrystallized from a mixed solvent of CHCl3 and benzene

Quellen und Nachweise

ORD-Eintrag
ord-acaa4dd7379e47b2a113b4193cc44c09
Quelldatensatz
uspto-grants-1984_05
Patentnummer
US04448962

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