関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Anthranilic Acid | HCID 227 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Benzoic acid, 2-(((4-methylphenyl)sulfonyl)amino)- | HCID 22763 | 83% |
反応手順
99.26 g of anthranilic acid was added to 830 g of water, the resulting mixture was heated at 75° C. and 165.3 g of p-toluenesulfonyl chloride was added thereto over 30 minutes with stirring. 495 g of 28% aqueous solution of sodium hydroxide was added dropwise and the mixture was stirred at 80° C. for one hour. The reaction mixture was added dropwise to a mixed solution of 360 g of 35% hydrochloric acid and 270 g of water at 70 to 80° C. and stirred for one hour. After cooling to 30° C., the mixture was filtered, the resulting crystals were washed with water, and the wet crystals were heated and solved in 750 g of 1-propanol to obtain a solution. After cooling to a room temperature, the solution was filtered, the resulting crystals were washed with 1-propanol, and dried under a reduced pressure to obtain 175 g of N-tosyl anthranilic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06852862B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-d6b42f002bf04ae1b1cd8f19a1bb7b9e |
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| 出典メモ | uspto-grants-2005_02 |
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