Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 130128 | HCID 130128 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 13960209 | HCID 13960209 | 82.7% |
Reaction Steps
1.87 g (0.005 mole) of 9-fluoro-5-methyl-8-(4-methyl-1-piperazinyl)-6,7-dihydro-1,7-dioxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid was dissolved, at room temperature, in a mixture of 25 ml of 2N aqueous solution of sodium hydroxide and 5 ml of ethanol. 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 ethanol. These crystals were recrystallized from water to obtain 1.77 g (82.7% yield) of 9-fluoro-5-methyl-8-(4-methyl-1-piperazinyl)-6,7-dihydro-1,7-dioxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid hydrochloride monohydrate in the form of yellow crystals. These crystals had a melting point of 225°-228° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04720495 |
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| Source dataset | uspto-grants-1988_01 |
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| ORD ID | ord-5dc56e230ebe414bbba41ae9603242f9 |
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| Source note | uspto-grants-1988_01 |
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