Acetic Acid → HCID 4914114, Verbindung

HRID 2291286Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2291286
C([NH:8][C:9]1[C:18]([F:19])=[C:17]([N:20]2[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]2)[C:16]([F:27])=[C:15]2[C:10]=1[C:11](=[O:34])[C:12]([C:31]([OH:33])=[O:32])=[CH:13][N:14]2[CH:28]1[CH2:30][CH2:29]1)C1C=CC=CC=1.C(O)(=O)C>[C].[Pd].C(O)C>[NH2:8][C:9]1[C:18]([F:19])=[C:17]([N:20]2[CH2:21][CH2:22][N:23]([CH3:26])[CH2:24][CH2:25]2)[C:16]([F:27])=[C:15]2[C:10]=1[C:11](=[O:34])[C:12]([C:31]([OH:33])=[O:32])=[CH:13][N:14]2[CH:28]1[CH2:30][CH2:29]1

Komponenten

5

Edukt 2

HCID 176Acetic AcidHCID 146641725-Benzylamino-1-cyclopropyl-6,8-difluoro-7-(4-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

Produkt 1

HCID 4914114HCID 4914114, VerbindungAusbeute 90,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 5-benzylamino-1-cyclopropyl-6,8-difluoro-7-(4-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (700 mg), 5% palladium-carbon (0.2 g), acetic acid (10 ml), and ethanol (15 ml) was stirred at room temperature for 30 minutes under a hydrogen stream. The catalyst was filtered off and the filtrate was evaporated under reduced pressure. After addition of water to the residue, the mixture was adjusted to pH 8 with aqueous ammonia. The resulting crystals were filtered to give 5-amino-1-cyclopropyl-6,8-difluoro-7-(4-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (510 mg), m.p. 254°-255° C.

Aufarbeitung

  1. filtrationThe catalyst was filtered off
  2. customthe filtrate was evaporated under reduced pressure
  3. additionAfter addition of water to the residue
  4. filtrationThe resulting crystals were filtered

Quellen und Nachweise

ORD-Eintrag
ord-0b78857c83e54f38971dac3414b8c17f
Quelldatensatz
uspto-grants-1989_01
Patentnummer
US04795751

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