HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Potassium Persulfate | HCID 24412 | — |
| Reactant | 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-4,5-dihydro-1H-pyrazole-5-carboxamide | HCID 44185606 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamide | HCID 66736193 | 90.3% |
Reaction Steps
0.24 g of potassium peroxodisulfate and 0.02 g of sulfuric acid were added to a N,N-dimethylformamide 3 ml solution comprising 0.10 g of 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-4,5-dihydro-1H-pyrazole-5-carboxamide, followed by reflux with heating. 1.5 hours later, the reaction liquid was stood to cool and poured to 10 ml of water, followed by extraction with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/0 to 1/2) to obtain 0.09 g of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08115006B2 |
| Source dataset | uspto-grants-2012_02 |
| ORD ID | ord-38d77f279aba41a08a51d70af16fb31e |
| Source note | uspto-grants-2012_02 |