HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 15021555, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Piperidinol, 1-methyl- | HCID 66048 | — |
| Reactant | 1-Ethyl-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid | HCID 800521 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 15021555 | HCID 15021555 | 9.9% |
Reaction Steps
To a mixture of 280 mg of 6,7-difluoro-1-ethyl-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 345 mg of N-methyl-4-piperidinol and 4 ml of DMF was added 200 mg of 50% sodium hydride while the former was stirred under ice cooling. After the resultant mixture was stirred for 2 hours at room temperature, 260 mg of acetic acid was added, followed by the addition of chloroform and water. The resultant mixture was thoroughly shaken and mixed. The chloroform layer was collected, washed with water, and then dried over sodium sulfate. The solvent was distilled off under reduced pressure. A solid thus precipitated was collected by filtration, whereby 38 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-52a2e0543ae546c3b134df7045c421ff |
| Source note | uspto-grants-1992_10 |