Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Hydroxylamine HCl | HCID 21645 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 86644482 | HCID 86644482 | — |
| Product | HCID 86644484 | HCID 86644484 | — |
Reaction Steps
Then, 0.43 g of 5-formyl-1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-3-{1,1,2-trifluoro-2-(trifluoromethoxy)ethoxy}pyrazole was dissolved in 15 mL of methanol, and 110 mg of sodium acetate and 90 mg of hydroxylammonium chloride were added, followed by stirring under reflux with heating for 2 hours. Then, the solvent was distilled off under reduced pressure, extraction with ethyl acetate was carried out, the organic layer was dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure, and the obtained residue was purified by column chromatography (developing solvent ethyl acetate:hexane=1:3) to obtain 0.29g of 1-{2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenyl}-5-(hydroxyimino)methylene-3-{1,1,2-trifluoro-2-(trifluoromethoxy)ethoxy}pyrazole (1H-NMR (CDCL3/TMS δ (ppm) value) 6: (majar) 2.55 (3H, s), 3.38 (2H, q), 6.05 (1H, dt), 6.54 (1H, s), 7.15 (1H, d), 7.61 (1H, d), 7.71 (1H, brs), 7.83 (1H, d)).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08802713B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-6b7e5734241c4698893c32f4eb7e2226 |
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| Source note | uspto-grants-2014_08 |
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