HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → 3-(1-ethyl-1H-pyrazol-5-yloxy)-5-(pyridin-2-ylthio)picolinonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 5-bromo-3-(1-ethyl-1H-pyrazol-5-yloxy)picolinonitrile | HCID 67485832 | — |
| Reactant | HCID 178418616 | HCID 178418616 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 3-(1-ethyl-1H-pyrazol-5-yloxy)-5-(pyridin-2-ylthio)picolinonitrile | HCID 67486233 | 93.3% |
Reaction Steps
5-Bromo-3-(1-ethyl-1H-pyrazol-5-yloxy)picolinonitrile (16.1 g, 55 mmol) and cesium carbonate (17.9 g, 55 mmol) were combined with DMF (160 ml) and pyridine-2-thiol (6.1 g, 55 mmol) dissolved in DMF (40 ml) was added dropwise over 30 minutes. The mixture was then agitated for 1 hour, quenched with saturated ammonium chloride solution and extracted with ethyl acetate. The combined organic extracts were washed with water and brine, dried (MgSO4), filtered and evaporated. The residue was purified over silica gel (20-35% ethyl acetate/hexanes) to afford 3-(1-ethyl-1H-pyrazol-5-yloxy)-5-(pyridin-2-ylthio)picolinonitrile (16.6 g, 93% yield) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08212045B2 |
| Source dataset | uspto-grants-2012_07 |
| ORD ID | ord-5491ce908d4f4dc1924d28c3a27d4e78 |
| Source note | uspto-grants-2012_07 |