関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 反応物 | 2-Octanol, 1,1,1-trifluoro- | HCID 97804 | — |
| 反応物 | 4-Benzyloxybenzoylchloride | HCID 3766410 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Benzoic acid, 4-(phenylmethoxy)-, 1-(trifluoromethyl)heptyl ester | HCID 14549213 | 61.2% |
反応手順
To a solution of 4-benzyloxybenzoic acid chloride (4.3 g) in methylene chloride (50 ml) was slowly added under ice cooling a solution of optically active 1,1,1-trifluoro-2-octanol (2.9 g), dimethylaminopyridine (0.6 g) and triethylamine (1.7 g) in methylene chloride (50 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 dried over anhydrous magesium sulfate. After the solution was distilled to remove the solvent, the crude product obtained was purified by silica-gel column chromatography and recrystallized from ethanol to obtain the titled compound (3.8 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-ec0352d8ee864b43808ea087b5fd241a |
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| 出典メモ | uspto-grants-1993_05 |
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