HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Peroxide → 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| 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 | 60.6% |
Reaction Steps
1.13 g of a 30% hydrogen peroxide solution was added to an ethyl acetate 12 ml solution comprising 0.53 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. 30 hours later, the reaction liquid was stood to cool and poured to 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=4/1) to obtain 0.32 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-576e9d3cf6644beeaa890b3285d9e027 |
| Source note | uspto-grants-2012_02 |