関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromo-4-(trifluoromethoxy)benzene | HCID 521008 | — |
| 反応物 | 4-(4-Hydroxybutoxy)phenol | HCID 22408055 | — |
| 生成物 | 4-(4-(Trifluoromethoxyphenoxy)phenoxy]butan-1-ol | HCID 22407856 | — |
反応手順
A mixture of 3.13 g of 4-(4-hydroxyphenoxy)butan-1-ol, 4.97 g of 4-(trifluoromethoxy)bromobenzene, and 4.75 g of K2CO3 are placed in a flask and flushed with N2 gas. To this are added 17 ml of pyridine and, after heating to 90° C., 3.42 g of CuO. The reaction mixture is heated at reflux for 2 days, and then cooled and poured into an ice/3N HCl mixture. This mixture is extracted twice with ether; and after separating, the combined ether extracts are washed with saturated NaHCO3, followed by brine, and then dried over MgSO4. Filtration and evaporation yields an oily residue which is purified by flash chromatography on silica gel, using 2:1 hexane/EtOAc as eluant. After evaporation, 4-[4-(4-(trifluoromethoxyphenoxy)phenoxy]butan-1-ol is obtained as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05412137 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-4e8cbc51bc67495bb37ccd36a1e86950 |
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| 出典メモ | uspto-grants-1995_05 |
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