HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Cesium carbonate → 4-tert-butyl-N-[5-chloro-2-(4-nitro-pyrazol-1-yl)-pyridin-3-yl]-benzenesulfonamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 4-nitro-1H-pyrazole | HCID 16376 | — |
| Edukt | trans-N,N'-dimethyl-1,2-cyclohexanediamine | HCID 2733821 | — |
| Edukt | N-(2-bromo-5-chloro-pyridin-3-yl)-4-tert-butyl-benzenesulfonamide | HCID 57942597 | — |
| Katalysator | Copper iodide | HCID 83717 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Lösungsmittel | Dimethylacetamide | HCID 31374 | — |
| Produkt | 4-tert-butyl-N-[5-chloro-2-(4-nitro-pyrazol-1-yl)-pyridin-3-yl]-benzenesulfonamide | HCID 68464085 | — |
Reaktionsschritte
A solution of N-(2-bromo-5-chloro-pyridin-3-yl)-4-tert-butyl-benzene sulfonamide (534 mg, 1.32 mmol), 4-nitropyrazole (224 mg, 1.98 mmol), trans-N,N′-dimethyl-cyclohexane-1,2-diamine (42 μL, 0.264 mmol), copper iodide (51 mg, 0.264 mmol), and cesium carbonate (903 mg, 2.77 mmol) in 5 mL of N,N-dimethylacetamide was heated at 130° C. for 2 hours. Ethyl acetate and water were added and the layers were separated. The organic layer was washed with brine, dried over magnesium sulfate, filtered, and concentrated in vacuo. The crude reside was subsequently purified by flash column chromatography (0-100% ethyl acetate in hexanes) to afford 4-tert-butyl-N-[5-chloro-2-(4-nitro-pyrazol-1-yl)-pyridin-3-yl]-benzenesulfonamide as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08835468B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-f9f0f6399497473a809f2b5cef77dd9d |
| Quellennotiz | uspto-grants-2014_09 |