HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → Ethyl 4-chloro-8-nitroquinoline-3-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Ethyl 8-nitro-4-oxo-3,4-dihydroquinoline-3-carboxylate | HCID 21250014 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | Ethyl 4-chloro-8-nitroquinoline-3-carboxylate | HCID 11196760 | 75% |
Reaction Steps
A mixture of 3-ethoxycarbonyl-8-nitro-4-oxo-3,4-dihydro-quinoline (10.2 g) and phosphorous oxychloride (10 ml) was stirred at reflux for 2 hours. The warm reaction mixture was added cautiously to a vigorously stirred mixture of ice, concentrated aqueous ammonia and chloroform. The organic layer was separated, washed with water, dried and evaporated to dryness. The residue was purified by flash chromatography on silica using chloroform as eluant to give 4-chloro-3-ethoxycarbonyl-8-nitro-quinoline in 75% yield, mp 253-254° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06200974B1 |
| Source dataset | uspto-grants-2001_03 |
| ORD ID | ord-2a149603b90f41c0b94a10774b68833a |
| Source note | uspto-grants-2001_03 |