Ethanol → HCID 68431852, Verbindung

HRID 1018537Notizen

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.[P:35](=[O:39])([OH:38])([OH:37])[OH:36]>O>[P:35]([OH:39])([OH:38])([OH:37])=[O:36].[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: 50 °C

Versuchsvorschrift

In 10 ml of 50% water-containing ethanol is suspended 0.5 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 the suspension is warmed to 50° C., after which 0.14 g of phosphoric acid is added to the warmed suspension to form a uniform solution. Subsequently, the solution is stirred at the same temperature for 10 minutes and then subjected to filtration. The filtrate is cooled to room temperature and then the crystals deposited are collected by filtration to obtain 0.32 g of (R)-1-cyclopropyl-8-difluoromethoxy-7-(1-methyl-2,3-dihydro-1H-5-isoindolyl)-4-oxo-1,4-dihydro-3-quinolinecarboxylic acid phosphate.

Aufarbeitung

customto form a uniform solution
filtrationsubjected to filtration
temperatureThe filtrate is cooled to room temperature
filtrationthe crystals deposited are collected by filtration

Quellen und Nachweise

ORD-Eintrag: ord-bee5593e633f4c81ad0c68fe951f40e4
Quelldatensatz: uspto-grants-2002_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06482835B2

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