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Triethylamine → 2-Chloro-N,N-dimethyl-5-nitrobenzene-1-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 反応物 | 2-Chloro-5-nitrobenzenesulfonyl chloride | HCID 20630 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-N,N-dimethyl-5-nitrobenzene-1-sulfonamide | HCID 20105580 | 73.8% |
反応手順
To a solution of 80 g of 2-chloro-5nitrobenzenesulfonyl chloride (Example A-1 above) in 200 ml of methylene chloride heated to reflux, was slowly added a solution of 30 g of dimethylamine hydrochloride in 30 ml of water followed by a dropwise addition of triethylamine. After completion of the addition, the reaction mixture was refluxed for 20 minutes, cooled to room temperature and concentrated by rotatory evaporation. The residue was treated with water and the resulting solid was filtered and recrystallized from ethanol, affording 61 g of the title compound, mp 138°-140° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05324854 |
| 出典データセット | uspto-grants-1994_06 |
| ORD ID | ord-4ce918f0fb2a4331846d12e3aad9e479 |
| 出典メモ | uspto-grants-1994_06 |