関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Chloro-2,4-Dinitrobenzene | HCID 6 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-chloro-N-methoxybenzenesulfonamide | HCID 18509319 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chloro-2',4'-dinitro-N-methoxybenzenesulfonanilide | HCID 18509309 | 62.6% |
反応手順
To a suspension of sodium hydride (60%, 0.09 g (2.25 mmol)) in DMF (3.0 ml), 2-chloro-N-methoxybenzenesulfonamide (0.48 g (2.17 mmol)) was added with stirring under cooling with ice. To the resulting mixture, after 15 minutes' stirring under cooling with ice, 2,4-dinitrochlorobenzene (0.41 g (2.02 mmol)) was added. The resulting mixture was then stirred under cooling with ice for one hour and at room temperature for one hour. Water was added to the reaction mixture and the resulting mixture was extracted with diethyl ether. The extract was washed with water, dilute hydrochloric acid and a saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure, to give 0.49 g (62%) of the title compound as pale yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06586617B1 |
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| 出典データセット | uspto-grants-2003_07 |
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| ORD ID | ord-417d9c004e9d4ddb915af227f99c2b35 |
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| 出典メモ | uspto-grants-2003_07 |
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