Sodium Hydroxide → Magnesium [5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate]

HRID 1648665Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1648665
[OH-].[Na+].[NH2:3][C:4]1[C:13]([F:14])=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:11]([O:22][CH:23]([F:25])[F:24])=[C:10]2[C:5]=1[C:6](=[O:32])[C:7]([C:29]([OH:31])=[O:30])=[CH:8][N:9]2[CH:26]1[CH2:28][CH2:27]1.[Cl-].[Mg+2:34].[Cl-]>>[NH2:3][C:4]1[C:13]([F:14])=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:11]([O:22][CH:23]([F:24])[F:25])=[C:10]2[C:5]=1[C:6](=[O:32])[C:7]([C:29]([O-:31])=[O:30])=[CH:8][N:9]2[CH:26]1[CH2:27][CH2:28]1.[Mg+2:34].[NH2:3][C:4]1[C:13]([F:14])=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:11]([O:22][CH:23]([F:24])[F:25])=[C:10]2[C:5]=1[C:6](=[O:32])[C:7]([C:29]([O-:31])=[O:30])=[CH:8][N:9]2[CH:26]1[CH2:27][CH2:28]1

Komponenten

4

Edukt 3

HCID 14798Sodium HydroxideHCID 5360315Magnesium ChlorideHCID 150238035-Amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

Produkt 1

HCID 21619245Magnesium [5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate]Ausbeute 90,4 %

Versuchsvorschrift

23.0 ml (0.0023 mole) of a 0.1N aqueous solution of sodium hydroxide were added to 1.00 g (0.00234 mole) of 5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (prepared as described in Example 30), and the resulting insoluble material was removed by filtration. 0.11 g (0.00115 mole) of anhydrous magnesium chloride was added to the filtrate, and the mixture was stirred at room temperature for 90 minutes. At the end of this time, the resulting precipitate was collected by filtration and washed with water, to give 0.91 g of magnesium [5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate] as a yellow powder, melting at 291°-293° C. (with decomposition).

Aufarbeitung

  1. customthe resulting insoluble material was removed by filtration
  2. filtrationAt the end of this time, the resulting precipitate was collected by filtration
  3. washwashed with water

Quellen und Nachweise

ORD-Eintrag
ord-5dec9d1b50864e04b339310291d16da6
Quelldatensatz
uspto-grants-1995_07
Patentnummer
US05436367

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