Citric Acid → HCID 68432751, Verbindung

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Reaktionsgleichung

C(O)C.[CH:4]1([N:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:21]4[CH:22]=[C:23]5[C:27](=[CH:28][CH:29]=4)[C@@H:26]([CH3:30])[NH:25][CH2:24]5)[C:15]=3[O:17][CH:18]([F:20])[F:19])[C:10](=[O:31])[C:9]([C:32]([OH:34])=[O:33])=[CH:8]2)[CH2:6][CH2:5]1.[C:35]([OH:47])(=[O:46])[CH2:36][C:37]([CH2:42][C:43]([OH:45])=[O:44])([C:39]([OH:41])=[O:40])[OH:38]>O>[C:35]([OH:47])(=[O:46])[CH2:36][C:37]([CH2:42][C:43]([OH:45])=[O:44])([C:39]([OH:41])=[O:40])[OH:38].[CH:4]1([N:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:21]4[CH:22]=[C:23]5[C:27](=[CH:28][CH:29]=4)[C@@H:26]([CH3:30])[NH:25][CH2:24]5)[C:15]=3[O:17][CH:18]([F:20])[F:19])[C:10](=[O:31])[C:9]([C:32]([OH:34])=[O:33])=[CH:8]2)[CH2:6][CH2:5]1

Komponenten

Reaktionsbedingungen

Temperatur: 65 °C

Versuchsvorschrift

In 42 ml of 50% water-containing ethanol is suspended 0.2 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid and 0.11 g of citric acid is then added thereto, after which the resulting mixture is warmed to 65° C. to form a uniform solution. Subsequently, the solution is filtered at the same temperature and the filtrate is concentrated, after which the crystals deposited are collected by filtration to obtain 0.24 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid citrate.

Aufarbeitung

additionis then added
customto form a uniform solution
filtrationSubsequently, the solution is filtered at the same temperature
concentrationthe filtrate is concentrated
filtrationafter which the crystals deposited are collected by filtration

Quellen und Nachweise

ORD-Eintrag: ord-18bafe62638547dc9b5daa65aabfa713
Quelldatensatz: uspto-grants-2002_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06482835B2

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