関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 2-Amino-4-methoxybenzoic acid | HCID 351010 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Iodo-4-methoxybenzoic acid | HCID 12822182 | 52% |
反応手順
A mixture of 4-methoxyanthranilic acid (30.5 g, 0.18 mol), water (274.5 ml), and concentrated HCl (36.6 ml) was heated at 75° C. to effect solution and then was cooled to 0° C. The mixture was then treated with NaNO2 (13.3 g) in water (27.5 ml), followed by potassium iodide (45.75 g) in a water (75 ml)/H2SO4 (10.1 ml) solution. The reaction mixture was heated on a steam bath for 2 hours, then excess iodine was steam distilled. The reaction mixture was then cooled and the product was collected by filtration and dried in an oven at 75° C. To afford 39.28 g (78.6%) of crude product. The crude product was treated with toluene, the mixture was filtered and the filtrate was concentrated to afford 26.03 g of 2-iodo-4-methoxybenzoic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06008226 |
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| 出典データセット | uspto-grants-1999_12 |
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| ORD ID | ord-593e53600721465ca80007ad82b445f8 |
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| 出典メモ | uspto-grants-1999_12 |
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