HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
HRID 448820Erstellt: 25. Oktober 2026
Sulfuric Acid → 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamide
https://huagongshe.com/reaction/448820
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Potassium Persulfate | HCID 24412 | — |
| Edukt | 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-4,5-dihydro-1H-pyrazole-5-carboxamide | HCID 44185606 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamide | HCID 66736193 | 90,3% |
Reaktionsschritte
0.24 g of potassium peroxodisulfate and 0.02 g of sulfuric acid were added to 3 ml of an N,N-dimethylformamide solution containing 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 heating and refluxing. After 1.5 hours, the reaction liquid was left to cool and introduced into 10 ml of water, and then ethyl acetate was added, followed by extraction. The organic layer (the ethyl acetate 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 (melting point: 231-233° C.).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08481744B2 |
|---|
| Quelldatensatz | uspto-grants-2013_07 |
|---|
| ORD ID | ord-5b2021305ef24e90aa308a488e79064a |
|---|
| Quellennotiz | uspto-grants-2013_07 |
|---|