Hydrochloric Acid → 7-(3-Amino-4-methyl-1-pyrrolidinyl)-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid hydrochloride

HRID 580577Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 580577
C(OC([NH:8][CH:9]1[CH:13]([CH3:14])[CH2:12][N:11]([C:15]2[C:24]([F:25])=[C:23]3[C:18]([C:19](=[O:32])[C:20]([C:29]([OH:31])=[O:30])=[CH:21][N:22]3[CH:26]3[CH2:28][CH2:27]3)=[CH:17][C:16]=2[F:33])[CH2:10]1)=O)(C)(C)C.[ClH:34]>CO>[ClH:34].[NH2:8][CH:9]1[CH:13]([CH3:14])[CH2:12][N:11]([C:15]2[C:24]([F:25])=[C:23]3[C:18]([C:19](=[O:32])[C:20]([C:29]([OH:31])=[O:30])=[CH:21][N:22]3[CH:26]3[CH2:28][CH2:27]3)=[CH:17][C:16]=2[F:33])[CH2:10]1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 139331017-(3-t-Butoxycarbonylamino-4-methyl-1-pyrrolidinyl)-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid

Produkt 1

HCID 139205727-(3-Amino-4-methyl-1-pyrrolidinyl)-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

7-(3-t-Butoxycarbonylamino-4-methyl-1-pyrrolidinyl)-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (0.27 g) was dissolved in a mixture of methanol (5 ml) and concentrated hydrochloric acid (5 ml) and stirred at room temperature for 30 minutes. After the reacting mixture was concentrated under reduced pressure, the resulting residue was dissolved in ethanol (10 ml) and crystallized with cooling. The resulting precipitate was recrystallized from methanol to give the title compound (0.14 g) as pale yellow powder, mp 272°-274° C.

Aufarbeitung

  1. concentrationAfter the reacting mixture was concentrated under reduced pressure
  2. dissolutionthe resulting residue was dissolved in ethanol (10 ml)
  3. customcrystallized
  4. temperaturewith cooling
  5. customThe resulting precipitate was recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-e9e3f3ea12494c86975d71e914709420
Quelldatensatz
uspto-grants-1988_06
Patentnummer
US04753953

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