Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| Reactant | HCID 178481841 | HCID 178481841 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86645105 | HCID 86645105 | 92% |
Reaction Steps
To a mixed solution of 4-[1,2-dihydro-1-methyl-2-oxo-6-(trifluoromethyl)pyridine-3-carbonyl]-5-hydroxy-1-methyl-1H-pyrazole (0.25 g, 0.80 mmol), pyridine (0.13 g, 1.6 mmol) and chloroform (5 mL), p-toluenesulfonyl chloride (0.23 g, 1.2 mmol) was added little at a time. After the stirring for a day at room temperature, the reaction mixture was poured into water and extracted with chloroform. The organic layer was washed with water, and dried over anhydrous magnesium sulfate. After separating the inorganic substance by filtration, the solvent was distilled off under reduced pressure, and thus obtained residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane=1/1.5), to obtain 0.33 g of a subject compound (yield: 92%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08076487B2 |
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| Source dataset | uspto-grants-2011_12 |
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| ORD ID | ord-07fb4bc23c9949a997f91e99b19aeec1 |
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| Source note | uspto-grants-2011_12 |
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