関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Tetrachloride | HCID 5943 | — |
| 反応物 | Trimethylsilyl iodide | HCID 85247 | — |
| 反応物 | 3-Benzyloxy-5-trifluoromethylthiophen | HCID 11184470 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Hydroxy-2-(trifluoromethyl)thiophene | HCID 11084273 | 74% |
反応手順
A mixture of 1G (7.75 g) and tetrachloromethane (50 ml) was treated with iodotrimethylsilane (12.30 ml) and heated to 60° C. for 12 hours. The reaction mixture was stirred at room temperature for 12 hours. Water (50 ml) was added and the resulting reaction mixture was extracted with dichloromethane three times. The combined organic phases were washed with water and dried. The crude reaction mixture was eluted through hexane (100 g/silica gel) to remove benzyliodide and then with diethyl ether. The etheral phases were concentrated and distilled in vacuo to give the product (3.33 g, 74%) having a boiling point of 65°-66° C. at 4 mm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05869426 |
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| 出典データセット | uspto-grants-1999_02 |
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| ORD ID | ord-5390bef8f83d469c87d4be81a5a5a2b1 |
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| 出典メモ | uspto-grants-1999_02 |
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