関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Chloro-N,N-diethylacetamide | HCID 16844 | — |
| 反応物 | 3-Trifluoromethyl-4'-hydroxy-alpha-ethylbenzhydrol | HCID 181876 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-(3-Trifluoromethylphenyl)-1-[4-(diethylcarbamoylmethoxy)-phenyl]-propan-1-ol | HCID 20207217 | — |
反応手順
14.8 g. 1-(3-trifluoromethylphenyl)-1-(4-hydroxyphenyl)-propan-1-ol, 7.6 g. of anhydrous potassium carbonate, 2 g. of potassium iodide, 8.2 g. of monochloroacetic acid diethylamide and 150 ml. of dry acetone are boiled for 5 hours, under stirring. The reaction mixture is cooled and the solvent is distilled off under reduced pressure. To the residue water is added and it is extracted with benzene. The benzene phase is shaken with water and subsequently a 5% aqueous sodium hydroxide solution and washed to neutral with water. It is dried over anhydrous sodium sulfate, filtered off and the solution is evaporated in vacuo. The solid residue is crystallized from a mixture of n-hexane and ethyl acetate. 17.6 g. of the named compound are obtained, melting at 83°-84° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04605785 |
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| 出典データセット | uspto-grants-1986_08 |
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| ORD ID | ord-7d338cd0b7ea4d9b862df2ab907ad556 |
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| 出典メモ | uspto-grants-1986_08 |
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