関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 1,2,3-Benzothiadiazole-7-carboxylic acid, methyl ester | HCID 179401 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,2,3-Benzothiadiazole-7-carboxylic acid | HCID 10921109 | — |
反応手順
100 g (0.51 mol) of 7-methoxycarbonylbenzo-1,2,3-thiadiazole are suspended in 1000 ml of water, and then 310 ml of 2N sodium hydroxide solution and 5 ml of dioxane are added. The reaction mixture is heated to 40° C., is stirred for 4 hours at that temperature and is then cooled to 10° C. A further 1000 ml of water are added and the batch is neutralised with 310 ml of 2N hydrochloric acid. The resulting precipitate is isolated by filtration, lightly dried in a current of air and then dissolved in tetrahydrofuran and the solution is dried over magnesium sulfate, filtered and concentrated. The crystals are suspended in hexane, isolated by filtration and dried.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05190928 |
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| 出典データセット | uspto-grants-1993_03 |
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| ORD ID | ord-5b24337a92d343fbbef2a65fcdae2f8d |
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| 出典メモ | uspto-grants-1993_03 |
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