Hydrochloric Acid → HCID 13960234, compound

HRID 2413971Notes

Reaction equation

HRID 2413971 reaction equation
[F:1][C:2]1[CH:14]=[C:12]2[C:13]3[N:8]([CH:9]=[C:10]([C:16]([OH:18])=[O:17])[C:11]2=[O:15])[CH:7]([CH3:19])[CH:6]=[CH:5][C:4]=3[C:3]=1[N:20]1[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]1.[ClH:27]>[OH-].[Na+].C(O)(C)C>[ClH:27].[F:1][C:2]1[CH:14]=[C:12]2[C:13]3[N:8]([CH:9]=[C:10]([C:16]([OH:18])=[O:17])[C:11]2=[O:15])[CH:7]([CH3:19])[CH:6]=[CH:5][C:4]=3[C:3]=1[N:20]1[CH2:21][CH2:22][N:23]([CH3:26])[CH2:24][CH2:25]1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 13960233HCID 13960233, compound

Product 1

HCID 13960234HCID 13960234, compoundYield 76%

Reagents, catalysts & solvents 2

HCID 3776IsopropanolSolventHCID 14798Sodium HydroxideSolvent

Procedure

1.79 g (0.005 mole) of 9-fluoro-5-methyl-8-(4-methyl-1-piperazinyl)-1-oxo-1H, 5H-benzo[ij]quinolizine-2-carboxylic acid was dissolved, at room temperature, in a mixture of 17 ml of 3N aqueous solution of sodium hydroxide and 5 ml of isopropanol. This solution was adjusted to pH 1 by the addition of concentrated hydrochloric acid under cooling with ice. The crystals which separated out were collected by filtration and successively washed with small volumes of water and isopropanol. These crystals were recrystallized from water to obtain 1.50 g (76.0% yield) of 9-fluoro-5-methyl-8-(4-methyl-1-piperazinyl)-1-oxo-1H, 5H-benzo[ij]quinolizine-2-carboxylic acid hydrochloride in the form of pale-yellow crystals. These crystals had a melting point of 193°-197° C. (dec.).

Workup

  1. temperatureunder cooling with ice
  2. customThe crystals which separated out
  3. filtrationwere collected by filtration
  4. washsuccessively washed with small volumes of water and isopropanol
  5. customThese crystals were recrystallized from water

Sources & evidence

ORD record
ord-7e427d2597174dee9415e5501a6f3a99
Source dataset
uspto-grants-1988_01
Patent number
US04720495

Reaction notes

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