HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 178469642, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 68480474 | HCID 68480474 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178469642 | HCID 178469642 | 48.3% |
Reaction Steps
Then, 1.0 g of ethyl-3-ethoxy-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}pyrazole-4-carboxylate was dissolved in 30 mL of dichloromethane, and 3.08 g of boron tribromide was added under cooling with ice, followed by stirring at room temperature for 12 hours. Then, 10 mL of a saturated aqueous solution of citric acid was added, extraction with ethyl acetate was carried out, the organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, and the obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:1) to obtain 0.45 g of ethyl-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-hydroxypyrazole-4-carboxylate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08802713B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-3736409e15de4c84bba1748821b5a0f8 |
| Source note | uspto-grants-2014_08 |