Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetate | HCID 175 | — |
| Reactant | HCID 13472993 | HCID 13472993 | — |
| Solvent | Hexamethylphosphoramide | HCID 12679 | — |
| Product | HCID 13044299 | HCID 13044299 | 55.1% |
Reaction Steps
A mixture of 3 g of 9-fluoro-8-bromo-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid, 5 g of 4-piperidineethylene acetate and 30 ml of hexamethylphosphoric triamide was heated at 160° C. on an oil bath for 6 hours. After completion of reaction, hexamethylphosphoric triamide was distilled off under reduced pressure, and to the residue was added ethyl acetate to precipitate crystals which then were recrystallized from dimethylformamide containing a small amount of dilute hydrochloric acid to give 0.87 g of 9-fluoro-8-(4-oxo-1-piperidyl)-5-methyl-6,7-dihydro-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylic acid. m.p. not lower than 300° C., white rhombic crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04399134 |
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| Source dataset | uspto-grants-1983_08 |
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| ORD ID | ord-f8842a62e14344bcb6397ee5e6722ab9 |
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| Source note | uspto-grants-1983_08 |
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