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Sodium Iodide → 1-Ethoxy-3-fluoro-5-iodobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Tosylchloramide | HCID 31388 | — |
| 反応物 | 3-Ethoxy-5-fluorophenylboronic Acid (contains varying amounts of Anhydride) | HCID 44558175 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Ethoxy-3-fluoro-5-iodobenzene | HCID 67324085 | — |
反応手順
(3-Ethoxy-5-fluorophenyl)boronic acid (2.5 g, 0.014 mol) was dissolved in THF (30 mL) and a solution of sodium iodide (4.1 g, 0.028 mol) in H2O (15 mL) was added followed by a solution of chloramine T (7.8 g, 0.1 mol) in H2O (15 mL). After 20 h stirring, the reaction mixture was extracted with diethylether (3×50 mL). The organic layers were combined and the solvent was evaporated. The resulting residue was triturated with hexanes (3×) and the hexanes layers were combined. The solvent was evaporated to yield 1-Ethoxy-3-fluoro-5-iodobenzene as an orange oil. The product was used in the next reaction step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09115147B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-17692c58c7e14a32ab5a47e646113e38 |
| 出典メモ | uspto-grants-2015_08 |