HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → HCID 22250101, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Ethyl 7-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate | HCID 178469609 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | HCID 22250101 | HCID 22250101 | — |
Reaction Steps
A mixture of ethyl 7-fluoro-4-hydroxyquinoline-3-carboxylate (4.7 g), anhydrous potassium carbonate (3.0 g), dimethyl sulphate (2.52 g) and butanone (200 ml) can be boiled under reflux for 14 hours. The solvent can be evaporated and the residue can be triturated with dichloromethane (150 ml). The mixture can be filtered and the filtrate evaporated to a small volume. Diethyl ether can be added, causing a solid to precipitate. The solid can be collected, washed with ether, dried and recrystallised from industrial methylated spirit to give the compound ethyl 7-fluoro-1-methyl-4-oxo-1,4-dihydroquinoline-3-carboxylate, m.p. 164° C.-166° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06562838B2 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-91feee2a353b4c45ad27e03f334cc15a |
| Source note | uspto-grants-2003_05 |