HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Acetate → HCID 14501361, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | ethyl (S)-10-(2,6-dimethyl-4-pyridinyl)-8,9-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylate | HCID 14501359 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 14501361 | HCID 14501361 | 51.8% |
Reaction Steps
A solution of 1.20 g ethyl (S)-10-(2,6-dimethyl-4-pyridinyl)-8,9-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylate in 15 ml 1M hydrochloric acid was heated at reflux for 2 hours. The reaction mixture was cooled, poured into sodium acetate solution and extracted with methylene dichloride. The extract was dried (sodium sulfate) and concentrated, and the residue was crystallized from methanol to give 0.58 g (S)-10-(2,6-dimethyl-4-pyridinyl)-8,9-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid as a colorless solid, m.p. 307°-310° C., [α]D25 =-39.1° (1% in chloroform).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04839355 |
| Source dataset | uspto-grants-1989_06 |
| ORD ID | ord-4f544419b7b4475cabbee7bf6f5bbe0a |
| Source note | uspto-grants-1989_06 |