Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 15712728 | HCID 15712728 | — |
| Product | HCID 15712730 | HCID 15712730 | 51.5% |
Reaction Steps
To 1-cyclopropyl-6-fluoro-7-(4-formyl-1-piperazinyl)-5-methyl-3-formyl-1,4-dihydro-4-oxoquinoline (1.2 g) is added 3N hydrochloric acid (15 ml) and the mixture is refluxed for 1 hour. After distilling off hydrochloric acid under reduced pressure, water is added to the resulting residue. The mixture is made weakly alkaline with saturated aqueous sodium hydrogen carbonate solution and extracted with chloroform. The chloroform layer is washed with water, dried over sodium sulfate, and the chloroform is distilled off under reduced pressure. The resulting residue is purified by silica gel column chromatography (eluent, chloroform → chloroform : methanol =50 : 1) and recrystallized from ethanol to give 1-cyclopropyl-6-fluoro-7-(1-piperazinyl)-5-methyl-3-formyl-1,4-dihydro-4oxoquinoline (0.57 g), as pale yellow powdery crystals, m.p. 21020 -213° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04971970 |
|---|
| Source dataset | uspto-grants-1990_11 |
|---|
| ORD ID | ord-b365ca8e66774c88bc59f27578e1695e |
|---|
| Source note | uspto-grants-1990_11 |
|---|