Hydrochloric Acid → HCID 13933100, compound

HRID 580575Notes

Reaction equation

HRID 580575 reaction equation
[C:1]([N:4]([CH:6]1[CH:10]([CH3:11])[CH2:9][N:8]([C:12]2[C:21]([F:22])=[C:20]3[C:15]([C:16](=[O:29])[C:17]([C:26]([OH:28])=[O:27])=[CH:18][N:19]3[CH:23]3[CH2:25][CH2:24]3)=[CH:14][C:13]=2[F:30])[CH2:7]1)C)(=O)C.[ClH:31]>>[ClH:31].[CH:23]1([N:19]2[C:20]3[C:15](=[CH:14][C:13]([F:30])=[C:12]([N:8]4[CH2:9][CH:10]([CH3:11])[CH:6]([NH:4][CH3:1])[CH2:7]4)[C:21]=3[F:22])[C:16](=[O:29])[C:17]([C:26]([OH:28])=[O:27])=[CH:18]2)[CH2:25][CH2:24]1

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 13933098HCID 13933098, compound

Product 1

HCID 13933100HCID 13933100, compound

Procedure

7-[3-(N-Acetyl-N-methylamino)-4-methyl-1-pyrrolidinyl]-1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-3-quinolinecarboxylic acid (0.56 g) was dissolved in 20% aqueous hydrochloric acid solution (5 ml) and refluxed for 2 hours. Then the reacting mixture was concentrated under reduced pressure, to the resulting residue was added ethanol (10 ml) and crystallized with cooling. The resulting precipitate was collected by filtration and recrystallized from methanol to give the title compound as pale yellow powder, mp 242°-246° C.

Workup

  1. temperaturerefluxed for 2 hours
  2. concentrationThen the reacting mixture was concentrated under reduced pressure, to the resulting residue
  3. additionwas added ethanol (10 ml)
  4. customcrystallized
  5. temperaturewith cooling
  6. filtrationThe resulting precipitate was collected by filtration
  7. customrecrystallized from methanol

Sources & evidence

ORD record
ord-48806f84494e480dbb042afd2c5dd6ae
Source dataset
uspto-grants-1988_06
Patent number
US04753953

Reaction notes

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