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Sodium Hydroxide → N-[3-(dimethylamino)phenyl]methanesulphonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | N,N-dimethyl-m-phenylenediamine | HCID 76084 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-[3-(dimethylamino)phenyl]methanesulphonamide | HCID 13796402 | 79% |
反応手順
Methanesulphonyl chloride (838 mg, 7.35 mmol) was added slowly to a cooled solution (5° C.) of N,N-dimethyl-1,3-phenylenediamine (1.00 g, 7.35 mmol) and sodium hydroxide (5M, 1.5 cm3) in water (10 cm3). The reaction was allowed to warm to room temperature overnight. The mixture was extracted with chloroform (3×15 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. Column chromatography (1:20 methanol/dichloromethane) gave the target material as a brown oil (1.24 g, 79%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08658665B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-b8fd1201b5654d798122c4747976812a |
| 出典メモ | uspto-grants-2014_02 |