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Sulfuric Acid → 2-Iodo-4-methoxybenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | 2-Amino-4-methoxybenzoic acid | HCID 351010 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Iodo-4-methoxybenzoic acid | HCID 12822182 | 60.1% |
反応手順
To a mixture of 50% sulfuric acid (150 ml) and 4-methoxyanthranilic acid (12 g) at 5°-10° C. was added sodium nitrite (5.5 g) in water, followed 10 minutes later by NaI (16.5 g) in water (30-50 ml). The reaction mixture was warmed to room temperature and stirred for 2 hours, then was heated at 60°-70° C. for 10 minutes, followed by stirring at room temperature for 1 hour. The reaction mixture was extracted with ether (4×125 ml) and the combined ether extracts were washed with water (50 ml×2), dried over MgSO4, filtered and evaporated. The residue was purified by column chromatography on silica gel eluting with ether to afford 12 g of 2-iodo-4-methoxybenzoic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05488055 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-ec526ee1a2af4b03a1b9c11234fdc2cf |
| 出典メモ | uspto-grants-1996_01 |