2-Methylpiperazine → HCID 13477665, Verbindung

HRID 370719Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 370719
Cl[C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:18])[C:7]([C:15]([OH:17])=[O:16])=[CH:8][N:9]2[CH2:12][CH2:13][F:14])=[CH:4][C:3]=1[F:19].[CH3:20][CH:21]1[CH2:26][NH:25][CH2:24][CH2:23][NH:22]1>N1C=CC=CC=1>[F:19][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:2]=1[N:25]1[CH2:24][CH2:23][NH:22][CH:21]([CH3:20])[CH2:26]1)[N:9]([CH2:12][CH2:13][F:14])[CH:8]=[C:7]([C:15]([OH:17])=[O:16])[C:6]2=[O:18]

Komponenten

4

Edukt 2

HCID 660572-MethylpiperazineHCID 127338801-(2-Fluoroethyl)-6-fluoro-7-chloro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

Produkt 1

HCID 13477665HCID 13477665, VerbindungAusbeute 33,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

A mixture of 1.50 g of 7-chloro-6-fluoro-1-(2-fluoroethyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 1.60 g of 2-methylpiperazine and 8 ml of pyridine was heated for 11 hours under reflux. The solvent of the reaction mixture was evaporated and the residue was dissolved in hot water. After cooling of the solution, the precipitate was filtered and recrystallized from ethanol to give 0.62 g of the title compound as colorless needles, M.p. 226°-227° C.

Aufarbeitung

  1. temperaturewas heated for 11 hours
  2. temperatureunder reflux
  3. customThe solvent of the reaction mixture was evaporated
  4. dissolutionthe residue was dissolved in hot water
  5. temperatureAfter cooling of the solution
  6. filtrationthe precipitate was filtered
  7. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-597460f404f646a3b0156df2060304f5
Quelldatensatz
uspto-grants-1985_07
Patentnummer
US04528287

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