化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Iodide → 2-Chloro-4-iodo-1-trifluoromethylbenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Sodium Thiosulfate | HCID 24477 | — |
| 反応物 | 3-Chloro-4-(trifluoromethyl)aniline | HCID 67962 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Chloro-4-iodo-1-trifluoromethylbenzene | HCID 66783212 | 73.4% |
反応手順
To a solution of 3-chloro-4-(trifluoromethyl)aniline (450 mg, 2.30 mmol) and toluene 4-sulfonic acid (1.19 g, 6.92 mmol) in CH3CN (10 mL) was added a solution of potassium iodide (955 mg, 5.76 mmol) and sodium nitrite (318 mg, 4.61 mmol) in water (1.8 mL) over 15 min at 10° C., then after 20 min the reaction mixture was poured onto water, neutralized with sat. aq. NaHCO3 solution, treated with 2 M aq. sodium thiosulfate solution (6 mL), and extracted with EtOAc. The organic layer was dried (MgSO4), filtered, and evaporated to afford the title compound (517 mg) as a light brown oil, which was directly used in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08138175B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-7ef7172636944e12b9986b5fd24a4f94 |
| 出典メモ | uspto-grants-2012_03 |