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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 mixture of 4-chloro-3-nitrobenzenesulfonamide (1 g), 4-methylpiperazin-1-amine dihydrochloride (1 g) and N1,N1,N2,N2-tetramethylethane-1,2-diamine (3 mL) in dioxane (10 mL) was refluxed for 12 hours, cooled to ambient temperature and filtered. The filtrate was added to a silica gel column (Analogix, SF65-200g) and purified by eluting with 1-5% methanol/dichloromethane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08563735B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-0529f5e247eb4fb586790e71eed884b1 |
| 出典メモ | uspto-grants-2013_10 |