Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | Levofloxacin q-acid | HCID 688333 | — |
| Solvent | Isobutanol | HCID 6560 | — |
| Product | Levofloxacin | HCID 149096 | 77.3% |
Reaction Steps
3 g (10.67 mmole) of (S)-(−)-9,10-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido [1,2,3-de] [1,4]benzoxazine-6-carboxylic acid was put in suspension in 21 mL of isobutanol and 4.75 mL (43 mmole) of N-methyl piperazine. The reaction mixture was heated to reflux for 6 hours, then slurried at ambient temperature for 60 hours and heated again to reflux for 7 hours until completion of the reaction. During that time, the reaction mixture became soluble at reflux temperature. The mixture was then cooled to 0° C., filtered under vacuum, washed with 7 mL isobutanol and 10 mL n-heptane, and dried overnight to obtain 2.83 g (77.3%) of levofloxacin.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07629458B2 |
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| Source dataset | uspto-grants-2009_12 |
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| ORD ID | ord-4ef587116a3a4c53b425d75c7f1018b3 |
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| Source note | uspto-grants-2009_12 |
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