HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 14846354, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Piperidinol, 1-methyl- | HCID 66048 | — |
| Reactant | 1-Cyclopropyl-6,7-difluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid | HCID 5210422 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 14846354 | HCID 14846354 | 80.3% |
Reaction Steps
To a mixture of 530 mg of 6,7-difluoro-1-cyclopropyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 690 mg of N-methyl-4-piperidinol and 8 ml of DMF was added 320 mg of 60% sodium hydride while the former was stirred under ice cooling. After the resultant mixture was stirred for 10 minutes at room temperature, 480 mg of acetic acid was added. DMF was distilled off under reduced pressure. To the residue was added 15 ml of n-hexane. The resultant mixture was thoroughly shaken and mixed. The supernatant was discarded. To the resultant precipitate was added 8 ml of ethanol, followed by stirring. A precipitate thus precipitated was collected by filtration, whereby 578 mg of the title compound was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05153203 |
| Source dataset | uspto-grants-1992_10 |
| ORD ID | ord-50e1a3dfdb904c6c8be673951f6d1590 |
| Source note | uspto-grants-1992_10 |