関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | (3,4-Dichlorophenyl)methanesulfonyl chloride | HCID 2794622 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (3,4-Dichlorophenyl)methanesulfonamide | HCID 20472420 | 81% |
反応手順
A solution of (3,4-dichloro-phenyl)-methanesulfonyl chloride (500 g, 1.93 mol) and acetone (470 mL) was added over 2 h to cooled (0-5° C.), stirred concentrated ammonium hydroxide (28%, 900 mL, 227 g NH3, 13.3 mol). The reaction mixture was maintained below 12° C. during the addition. The reaction mixture was allowed to warm to room temperature and was stirred for 1 h. Water (900 mL) was added to the reaction mixture and it was stirred for 1 h. The white solid was collected by filtration, washed with cold water (2×500 mL), and vacuum dried to give 375 g (81%) of (3,4-dichloro-phenyl)-methanesulfonamide with 99% purity (as determined by HPLC).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07582772B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-f0507f5963ea426db87d7ffd1d49254e |
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| 出典メモ | uspto-grants-2009_09 |
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