化工社化工社 化学情報印刷レポート · 研究参考用
Iodine → 2-Amino-3-fluoro-5-iodobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Amino-3-fluorobenzoic acid | HCID 586408 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Amino-3-fluoro-5-iodobenzoic acid | HCID 57731463 | 63% |
反応手順
To a solution of 999 mg (6.44 mmol) of 2-amino-3-fluorobenzoic acid in 35 mL of water was added 500 mg (5.95 mmol) of sodium bicarbonate. The reaction was stirred and 1.77 g (6.99 mmol) of iodine was slowly added. The reaction was stirred at room temperature for 48 hours. To the solution was added an aqueous solution of sodium bisulfite and the solution was stirred vigorously for 30 minutes. The precipitate was collected by vacuum filtration and washed with water. The brown solid was dried overnight to afford 1.14 g (4.06 mmol, 63% yield) of 2-amino-3-fluoro-5-iodo-benzoic acid. 1H NMR (500 MHz, DMSO-d6) δ 7.79 (t, 1H), 7.58 (dd, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07709645B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-f3e736818c964dad979f240d484d63f6 |
| 出典メモ | uspto-grants-2010_05 |