HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86700044, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2,2,2-Trifluoroethyl trifluoromethanesulfonate | HCID 80366 | — |
| Reactant | HCID 12624209 | HCID 12624209 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86700044 | HCID 86700044 | — |
Reaction Steps
Ethyl 4-oxo-5-phenyl-1,4-dihydropyridine-3-carboxylate (100 mg) was suspended in DMF (1.5 ml). Cesium carbonate (268 mg) and 2,2,2-trifluoroethyl trifluoromethanesulfonate (83 μl) were sequentially added and the mixture was stirred at room temperature for three hours. A 1 N aqueous hydrochloric acid solution was added under ice cooling, followed by extraction with ethyl acetate. The organic layer was washed with water and brine and then dried over sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography [chloroform:methanol=300:1->40:1 (v/v)] to give 159 mg of the title compound as an oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08933103B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-b1d3705f898141398bcb8bdba997eb28 |
| Source note | uspto-grants-2015_01 |