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Triethylamine → 7-[(3R)-3-(1-Aminocyclopropyl)-1-pyrrolidinyl]-6-fluoro-1-[(1R,2S)-2-fluorocyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid

HRID 1458010
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1458010
C(O[C:9]([N:11]1[CH2:15][CH2:14][C@@H:13]([C:16]2([NH:19]C(OC(C)(C)C)=O)[CH2:18][CH2:17]2)[CH2:12]1)=O)C1C=CC=CC=1.C(N(CC)CC)C.[F:34][C:35]1[CH:36]=[C:37]2[C:42](=[CH:43]C=1F)[N:41]([C@@H:46]1[CH2:48][C@@H:47]1[F:49])[CH:40]=[C:39]([C:50]([OH:52])=[O:51])[C:38]2=[O:53].[OH-].[Na+]>CO.[C].[Pd]>[NH2:19][C:16]1([C@@H:13]2[CH2:14][CH2:15][N:11]([C:9]3[CH:43]=[C:42]4[C:37]([C:38](=[O:53])[C:39]([C:50]([OH:52])=[O:51])=[CH:40][N:41]4[C@@H:46]4[CH2:48][C@@H:47]4[F:49])=[CH:36][C:35]=3[F:34])[CH2:12]2)[CH2:17][CH2:18]1
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Komponenten

7

Edukt 4

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 11132144(3R)-1-Benzyloxycarbonyl-3-(1-tert-butoxycarbonylaminocyclopropyl)pyrrolidineHCID 138524206,7-Difluoro-1-(cis-2-fluorocyclopropyl)-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

Produkt 1

HCID 69138374
7-[(3R)-3-(1-Aminocyclopropyl)-1-pyrrolidinyl]-6-fluoro-1-[(1R,2S)-2-fluorocyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid
Ausbeute 77 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysator2×HCID 887MethanolLösungsmittel

Versuchsvorschrift

A 322 mg (0.89 mmol) portion of (3R)-1-benzyloxycarbonyl-3-(1-tert-butoxycarbonylaminocyclopropyl)pyrrolidine was dissolved in 10 ml of methanol to which was subsequently added 100 mg of 5% palladium-carbon to carry out 2 hours of hydrogenation under normal pressure with warming by an infrared lamp. After completion of the reaction, 5% palladium-carbon was removed by filtration and methanol was evaporated. The resulting residue was dissolved in 5 ml of acetonitrile to which were subsequently added 0.5 ml of triethylamine and 113 mg (0.4 mmol) of 6,7-difluoro-[(1R,2S)-2-fluorocyclopropyl]-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, followed by 18 hours of heating under reflux. After completion of the reaction, the reaction solution was spontaneously cooled to collect the thus formed crystals by filtration. With cooling in an ice bath, to the thus obtained crystals was added dropwise 5 ml of concentrated hydrochloric acid, followed by 30 minutes of stirring at the same temperature. After completion of the reaction, the reaction solution was adjusted to pH 12 with sodium hydroxide aqueous solution and then to pH 7.4 with hydrochloric acid, followed by extraction with chloroform (50 ml×3). The organic layers were combined and dried on sodium sulfate, and then the solvent was evaporated. Thereafter, the resulting residue was recrystallized from liquid ammonia-ethanol to yield 120 mg (77%) of the title compound.

Aufarbeitung

  1. temperaturewith warming by an infrared lamp
  2. customwas removed by filtration and methanol
  3. customwas evaporated
  4. dissolutionThe resulting residue was dissolved in 5 ml of acetonitrile to which
  5. waitfollowed by 18 hours
  6. temperatureof heating
  7. temperatureunder reflux
  8. customAfter completion of the reaction
  9. temperaturethe reaction solution was spontaneously cooled
  10. customto collect the thus formed crystals
  11. filtrationby filtration
  12. temperatureWith cooling in an ice bath, to the thus obtained crystals
  13. additionwas added dropwise 5 ml of concentrated hydrochloric acid
  14. waitfollowed by 30 minutes
  15. customAfter completion of the reaction
  16. extractionto pH 7.4 with hydrochloric acid, followed by extraction with chloroform (50 ml×3)
  17. customdried on sodium sulfate
  18. customthe solvent was evaporated
  19. customThereafter, the resulting residue was recrystallized from liquid ammonia-ethanol

Quellen und Nachweise

ORD-Eintrag
ord-70deb89cb5b8465a927d559f98691242
Quelldatensatz
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05849757

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