関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloride | HCID 312 | — |
| 反応物 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 反応物 | 4-Benzyloxybenzoylchloride | HCID 3766410 | — |
| 反応物 | 1,1,1-Trifluorodecan-2-ol | HCID 3864464 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Benzoic acid, 4-(phenylmethoxy)-, 1-(trifluoromethyl)nonyl ester | HCID 14745753 | 96.3% |
反応手順
To a solution of 4-benzyloxybenzoic acid chloride (1.23 g) in methylene chloride (10 ml) was slowly added under ice cooling a solution of optically active 1,1,1-trifluoro-2-decanol (0.96 g), dimethylaminopyridine (0.55 g) and triethylamine (0.48 g) in methylane chloride (20 ml). The mixture was left to stand until it reached room temperature and allowed to react overnight. The mixture was poured in ice water and extracted with methylene chloride. The extracted layer was washed with dilute aqueous hydrochloric acid solution, water, 1N aqueous sodium carbonate solution and water in this order, and was dried over anhydrous magnesium sulfate. After the solution was distilled to remove the solvent, the crude product thus obtained was purified by toluene-silica-gel column chromatography and recrystallized from ethanol to obtain the titled compound (1.84 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05207947 |
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| 出典データセット | uspto-grants-1993_05 |
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| ORD ID | ord-859e072770fa41648e889dcb531ae8cb |
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| 出典メモ | uspto-grants-1993_05 |
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