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Sulfuric Acid → 2-Iodo-4-(trifluoromethoxy)phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | p-(Trifluoromethoxy)phenol | HCID 70015 | — |
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Iodo-4-(trifluoromethoxy)phenol | HCID 2769411 | 94% |
反応手順
To a suspension of N-iodosuccinimide (6.95 g, 31 mmol) in glacial acetic acid (2 ml) was added 4-trifluoromethoxy phenol (4.0 ml, 31 mmol) and, after 5 minutes, concentrated sulphuric acid (0.5 ml, 9 mmol). The pale brown suspension was stirred at room temperature under nitrogen for 48 hours before diluting with water and extracting with dichloromethane. Organic extract was washed with water, saturated aqueous sodium thiosulphate solution, water, dried over magnesium sulfate and decolourising charcoal added. The resulting suspension was left to stand for 30 minutes before filtering through a short pad of silica gel eluting with dichloromethane. The solvent was evaporated in vacuo to give the title compound as an oil, 8.78 g, 94% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541588B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-ed5b836a8b304d37a4e16c36dca41b8e |
| 出典メモ | uspto-grants-2013_09 |