1433857-09-0 → HCID 71570094, compound

HRID 1528025Notes

Reaction equation

HRID 1528025 reaction equation
[ClH:1].[CH:2]1([NH:5][CH2:6][C@@H:7]2[C@H:11]([F:12])[CH2:10][N:9]([C:13]3[C:22]([O:23][CH3:24])=[C:21]4[C:16]([C:17](=[O:31])[C:18]([C:28]([OH:30])=[O:29])=[CH:19][N:20]4[CH2:25][CH2:26][F:27])=[CH:15][C:14]=3[F:32])[CH2:8]2)[CH2:4][CH2:3]1>O>[OH2:23].[ClH:1].[CH:2]1([NH:5][CH2:6][C@@H:7]2[C@H:11]([F:12])[CH2:10][N:9]([C:13]3[C:22]([O:23][CH3:24])=[C:21]4[C:16]([C:17](=[O:31])[C:18]([C:28]([OH:30])=[O:29])=[CH:19][N:20]4[CH2:25][CH2:26][F:27])=[CH:15][C:14]=3[F:32])[CH2:8]2)[CH2:3][CH2:4]1

Participants

3

Reactant 1

HCID 715287671433857-09-0

Product 1

HCID 71570094HCID 71570094, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

0.3 mL of hot water at 70° C. was added to 0.02 g (0.04 mmol) of the 7-{(3S,4S)-3-[(cyclopropylamino)methyl]-4-fluoropyrrolidine-1-yl}-6-fluoro-1-(2-fluoroethyl)-8-methoxy-4-oxo-1,4-dihydroquinoline-3-carboxylic acid hydrochloride salt obtained in Reference Example 1 to dissolve the hydrochloride salt. The solution was allowed to cool to room temperature and left to stand overnight at 5° C. Precipitated crystals were filtrated and dried under reduced pressure to obtain a white powder of 7-{(3S,4S)-3-[(cyclopropylamino)methyl]-4-fluoropyrrolidine-1-yl}-6-fluoro-1-(2-fluoroethyl)-8-methoxy-4-oxo-1,4-dihydroquinoline-3-carboxylic acid hydrochloride salt hydrate (crystals C).

Workup

  1. customobtained in Reference Example 1
  2. waitleft
  3. customPrecipitated crystals
  4. filtrationwere filtrated
  5. customdried under reduced pressure

Sources & evidence

ORD record
ord-58a66fcd150e43f5a97390578f4fcca3
Source dataset
uspto-grants-2015_07
Patent number
US09090587B2

Reaction notes

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