関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 4-Methyl-3-sulfamoylbenzoic acid | HCID 239585 | — |
| 反応物 | Potassium Permanganate | HCID 516875 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Aminosulfonyl)-1,4-benzenedicarboxylic Acid | HCID 12802657 | — |
反応手順
To a solution of 44 g of 3-(aminosulfonyl)-4-methyl benzoic acid (Example 1) in 500 ml H2O was added 11.0 g of sodium carbonate and 72 g of potassium permanganate in 8 g portions at 50°-60° over 5.5 hours. Then, 1 ml formic acid was added to decompose excess oxidant and the solution was filtered hot (60°) through Celite. The filter pad was washed with hot water. The combined filtrate was concentrated, in vacuo to approximately 300 ml and brought to pH 6 with concentrated HCl. A small amount of solid was filtered off. The filtrate was brought to pH 3.5 with concentrated HCl. The resulting solid was collected, washed with water and dried to give 33 g of solid; m.p. 259-290 (known m.p. 312-314). This material was used, without further purification, in Example 3.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04302241 |
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| 出典データセット | uspto-grants-1981_11 |
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| ORD ID | ord-cfbb1be409114a27ba9f382e75f00e86 |
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| 出典メモ | uspto-grants-1981_11 |
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