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Methylamine → N-Methyl-4-nitrobenzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | 4-Nitrobenzenesulfonyl chloride | HCID 7404 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | N-Methyl-4-nitrobenzenesulfonamide | HCID 232993 | 98.4% |
反応手順
To a suspension of 4-nitrobenzenesulfonyl chloride (5 g, 22.56 mmol) in ether (250 ml), methylamine (5 ml, 40% aq. solution, 56.4 mmol) was added, and the mixture was stirred at room temperature. After 16 hr. the reaction mixture was concentrated to remove the solvent and the residue was resuspended in methylene chloride. After washing with 2N HCl and brine, the organic fractions were dried (MgSO4), filtered and concentrated to give N-methyl-4-nitrobenzenesulfonamide (4.8 g, 98%): mp (DSC) 109° C. Anal Calc'd. for C7H8N2O4S: C, 38.89; H, 3.73; N, 12.96. Found: C, 38.83; H, 3.72; N, 12.96.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07420061B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-ccb6d66ead81471897de02c5abc5b139 |
| 出典メモ | uspto-grants-2008_09 |