関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (R)-(+)-1,1,1-Trifluoro-2-octanol | HCID 2779099 | — |
| 反応物 | 4-Benzyloxybenzoylchloride | HCID 3766410 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (R)-(+)-1,1,1-trifluoro-2-octyl 4-benzyloxybenzoate | HCID 22850730 | 65.1% |
反応手順
To 5 ml of a methylene chloride solution containing 0.56 g of 4-benzyloxybenzoic acid chloride was slowly added a solution of 0.38 g of (R)-(+)-1-trifluoromethylheptanol and 0.23 g of triethylamine in 5 ml of methylene chloride under ice-cooling. The mixture was allowed to warm to room temperature and stirred at that temperature for 12 hours. The reaction mixture was poured into ice-water and extracted with methylene chloride. The methylene chloride phase was washed successively with diluted hydrochloric acid, water, an aqueous 1N sodium carbonate solution, and water and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and the residual crude product was purified by silica gel column chromatography to obtain 0.53 g of (R)-(+)-4-benzyloxybenzoic acid 1-trifluoromethylheptyl ester.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05110497 |
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| 出典データセット | uspto-grants-1992_05 |
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| ORD ID | ord-58a09efc368340d4a7a3508279458c22 |
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| 出典メモ | uspto-grants-1992_05 |
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