Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 22714642 | HCID 22714642 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 12993965 | HCID 12993965 | 65.3% |
Reaction Steps
2 g of phosphorus oxychloride were added dropwise to a mixture of 1 g of 2-(3,4,4-trifluoro-3-butenylthio)oxazolidin-4-one and 0.35 g of pyridine under ice cooling and stirred at 70-80° C. for 3 hours. After addition of ice water to the reaction mixture and stirring for 30 minutes, the mixture was extractred with dichloromethane. The extracted layer was washed with water, dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by column chromatography (eluent: dichloromethane) to obtain 0.7 g of 4-chloro-2-(3,4,4-trifluoro-3-butenylthio)oxazole (yield 65%). n20D=1.4813.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06743814B2 |
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| Source dataset | uspto-grants-2004_06 |
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| ORD ID | ord-bd2bdec8b51948b2856c769820f7d5b2 |
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| Source note | uspto-grants-2004_06 |
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