HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → N-[4-(5-cyano-1-methyl-1H-pyrrol-2-yl)-3-fluorophenyl]methanesulfonamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Methanesulfonyl chloride | HCID 31297 | — |
| Edukt | 5-(4-amino-2-fluorophenyl)-1-methyl-1H-pyrrole-2-carbonitrile | HCID 16050432 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | N-[4-(5-cyano-1-methyl-1H-pyrrol-2-yl)-3-fluorophenyl]methanesulfonamide | HCID 16051367 | 68,2% |
Reaktionsschritte
5-(4-amino-2-fluorophenyl)-1-methyl-1H-pyrrole-2-carbonitrile (0.20 g, 0.93 mmol) was dissolved in pyridine (2.0 mL). Methanesulfonyl chloride (0.07 mL, 0.9 mmol) was added and the mixture was stirred for 16 hours, followed by the addition of water. The mixture was diluted with ethyl acetate and then was washed with water, saturated CuSO4, 2N HCl, brine, dried over MgSO4, and concentrated. The crude product was purified via Isco chromatography (the Redisep® column, silica, gradient 5-50% ethyl acetate in hexane) to afford 0.18 g of N-[4-(5-cyano-1-methyl-1H-pyrrol-2-yl)-3-fluorophenyl]methanesulfonamide.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07291643B2 |
| Quelldatensatz | uspto-grants-2007_11 |
| ORD ID | ord-6d57220428844858a634e9d48cc56d37 |
| Quellennotiz | uspto-grants-2007_11 |