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Iodine → 4-Chloro-2-iodophenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Chlorophenol | HCID 4684 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Chloro-2-iodophenol | HCID 620234 | 7% |
反応手順
To a solution of 4-chlorophenol in THF (75 mL), and H2O (75 mL) was added a mixture of crushed iodine (78.7 mmol, 20 g) and sodium bicarbonate (78.7 mmol, 6.6 g). The reaction mixture was stirred at room temperature overnight, then quenched with sufficient 5% sodium thiosulfate solution to turn the color of the reaction mixture from deep violet to light yellow and extracted with ether (2×200 mL). The ether layer was collected, washed with H2O, and the washed ether layer was dried, filtered and the filtrate was evaporated to a crude product, which was purified by distillation to obtain 4-chloro-2-iodo phenol (7%, 1.3 g); mp 79° C.-82° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06849629B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-377ea90ca4ef427b88176d5de2f9524e |
| 出典メモ | uspto-grants-2005_02 |