化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → Benzoic acid, 4-(phenylmethoxy)-, 1-(trifluoromethyl)heptyl ester
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 | (R)-(+)-1,1,1-Trifluoro-2-octanol | HCID 2779099 | — |
| 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 added drop by drop a solution of (R)-(+)-1,1,1-trifluoro-2-octanol (2.9 g), dimethylaminopyridine (0.6 g) and triethylamine (1.7 g) in methylene chloride (50 ml), under ice cooling. The mixture was left to stand at the room temperature for 24 hours before being poured in ice water. The methylene chloride layer separated was washed with diluted hydrochloric acid, water 1N aqueous sodium carbonate solution and water in this order, dried over magnesium sulfate and distilled to obtain a crude objective compound. The compound was purified by toluene/silica gel chromatography and recrystallization from ethanol to obtain the titled compound (3.8 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05424005 |
| 出典データセット | uspto-grants-1995_06 |
| ORD ID | ord-b0bbf4059f3f4f6985f90088f6ed8e04 |
| 出典メモ | uspto-grants-1995_06 |