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Triethylamine → Benzenesulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | N,N-Bis(2-hydroxyethyl)-4-methylbenzenesulfonamide | HCID 81565 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Benzenesulfonamide | HCID 7370 | 85.7% |
反応手順
A solution of 11.4 g (0.1 mole) of methanesulfonyl chloride in 17.1 ml of dichloromethane is cooled to 5° C. A solution of 13 g (0.05 mole) of N,N-bis(2-hydroxyethyl)-4-methylbenzenesulfonamide and 10.1 g (0.1 mole) of triethylamine in 52 ml of dichloromethane is then added dropwise with stirring. The resulting mixture is allowed to return to ambient temperature and stirred for a further 3 hours. The reaction mixture is then extracted three times with 40 ml water. The organic phase is dried over sodium sulfate, filtered and concentrated in a rotating evaporator. The resulting oil is then crystallized from ethanol. 17.8 g of 4-methyl-N,N-bis[2-methylsulfonyloxy)ethyl]benzenesulfonamide are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05792770 |
| 出典データセット | uspto-grants-1998_08 |
| ORD ID | ord-ccc72a90f7184e26b8ea2436581a081a |
| 出典メモ | uspto-grants-1998_08 |