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Methylamine → 1-(5-Amino-2,4-difluorophenyl)-6-fluoro-5,8-dimethyl-7-methylamino-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid

HRID 369285
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 369285
[CH3:1][NH2:2].[NH2:3][C:4]1[C:5]([F:29])=[CH:6][C:7]([F:28])=[C:8]([N:10]2[C:19]3[C:14](=[C:15]([CH3:23])[C:16]([F:22])=[C:17](F)[C:18]=3[CH3:20])[C:13](=[O:24])[C:12]([C:25]([OH:27])=[O:26])=[CH:11]2)[CH:9]=1>N1C=CC=CC=1>[NH2:3][C:4]1[C:5]([F:29])=[CH:6][C:7]([F:28])=[C:8]([N:10]2[C:19]3[C:14](=[C:15]([CH3:23])[C:16]([F:22])=[C:17]([NH:2][CH3:1])[C:18]=3[CH3:20])[C:13](=[O:24])[C:12]([C:25]([OH:27])=[O:26])=[CH:11]2)[CH:9]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 155184811-(3-amino-4,6-difluorophenyl)-6,7-difluoro-5,8-dimethyl-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid

Produkt 1

HCID 232847851-(5-Amino-2,4-difluorophenyl)-6-fluoro-5,8-dimethyl-7-methylamino-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

Pyridine (300 mg) and a 40% aqueous solution (150 mg) of methylamine were added to 1-(5-amino-2,4-difluorophenyl)-6,7-difluoro-5,8-dimethyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (110 mg), and the mixture was heated and stirred at 40° C. for 8 days. The solvent and the like were distilled off under reduced pressure, and ethanol (0.5 ml) was added to the residue. The mixture was left to stand for 3 days, and solids deposited were collected by filtration and washed with ethanol and diethyl ether to obtain the title compound (20 mg) as a pale yellow powder.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. distillationThe solvent and the like were distilled off under reduced pressure, and ethanol (0.5 ml)
  3. additionwas added to the residue
  4. waitThe mixture was left
  5. waitto stand for 3 days
  6. filtrationsolids deposited were collected by filtration
  7. washwashed with ethanol and diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-8c4420c2d4d742018160f6f143d7d67c
Quelldatensatz
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06136823

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