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4-Chloro-3-nitrobenzenesulfonamide → 4-(4-Methylpiperazin-1-ylamino)-3-nitrobenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloro-3-nitrobenzenesulfonamide | HCID 7324 | — |
| 反応物 | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| 反応物 | 4-Methylpiperazin-1-ylamine dihydrochloride hydrate | HCID 198221 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(4-Methylpiperazin-1-ylamino)-3-nitrobenzenesulfonamide | HCID 4737741 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09034875B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-254c940763bb446c9c0bf28987f0e297 |
| 出典メモ | uspto-grants-2015_05 |