HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4-Chloro-3-nitrobenzenesulfonamide → 4-(4-Methylpiperazin-1-ylamino)-3-nitrobenzenesulfonamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4-Chloro-3-nitrobenzenesulfonamide | HCID 7324 | — |
| Edukt | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| Edukt | 4-Methylpiperazin-1-ylamine dihydrochloride hydrate | HCID 198221 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Produkt | 4-(4-Methylpiperazin-1-ylamino)-3-nitrobenzenesulfonamide | HCID 4737741 | — |
Reaktionsschritte
A 50 mL round-bottomed flask was charged with 4-chloro-3-nitrobenzenesulfonamide (1 g, 4.23 mmol), 4-methylpiperazin-1-amine dihydrochloride (1 g, 5.32 mmol), and N1,N1,N2,N2-tetramethylethane-1,2-diamine (3 mL, 20.01 mmol) in dioxane (10 mL). The reaction mixture was refluxed for 12 hours. After this time, the reaction mixture was cooled to room temperature, the salt filtered off via a Buchner funnel, and the solvent removed in vacuo. The crude product was added to a silica gel column (Analogix, SF65-200 g) and purified by eluting with 0-5% methanol in dichloromethane.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09034875B2 |
| Quelldatensatz | uspto-grants-2015_05 |
| ORD ID | ord-254c940763bb446c9c0bf28987f0e297 |
| Quellennotiz | uspto-grants-2015_05 |