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Iodine → 2-Iodo-4-(trifluoromethyl)phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | 4-(Trifluoromethyl)phenol | HCID 67874 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Thiourea | HCID 2723790 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Iodo-4-(trifluoromethyl)phenol | HCID 11572816 | — |
反応手順
A mixture of iodine (91.6 mmol, 23.2 g) and sodium bicarbonate (91.6 mmol, 7.7 g) was added to a solution of α,α,α-trifluoro-p-cresol (83.3 mmol, 13.5 g) in THF (90 mL) and H2O (90 mL) and the reaction mixture was allowed to stand at room temperature overnight. Sufficient thiourea (5% solution) was added to remove the excess iodine as indicated by the color change of the reaction from deep violet to brown. The reaction mixture was extracted with ether (3×100 mL), the extract was dried, filtered and the filtrate was concentrated to obtain a brown oil. This oil was distilled (bp 105° C. at 44 mm Hg) to obtain α,α,α-trifluoro-o-iodo-p-cresol (4.1 g, 75% pure, admixed with the starting α,α,α-trifluoro-p-cresol).
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-272e7eff9e6b4c39bef402449fd68506 |
| 出典メモ | uspto-grants-2005_02 |