Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 19993702 | HCID 19993702 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19993699 | HCID 19993699 | 55.5% |
Reaction Steps
A mixture of (RS)-3-carbamoyl-4-(2-chloro-1,1,2-trifluoroethoxy)-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole (0.75g) and phosphorus oxychloride (15ml) was heated at 80° C. for 6 hours. Water (100ml) and dichloromethane (50ml) were added to the cooled mixture and the layers were separated. The aqueous layer was extracted with dichloromethane (2x50ml) and the combined organic layers were washed with aqueous sodium hydrogen carbonate solution (1M; 30ml), dried over magnesium sulfate, and evaporated to give (RS)-4-(2-chloro-1,1,2-trifluoroethoxy)-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyanopyrazole (0.4g) as an off-white crystalline solid, m.p. 99°-101° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05055482 |
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| Source dataset | uspto-grants-1991_10 |
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| ORD ID | ord-ef51c71e917a45d2aaad982ed610f0af |
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| Source note | uspto-grants-1991_10 |
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