化工社化工社 化学情報印刷レポート · 研究参考用
Ethanol → Ethyl 4-methyl-3-(trifluoromethyl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 4-Methyl-3-(trifluoromethyl)benzoic acid | HCID 2775592 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Ethyl 4-methyl-3-(trifluoromethyl)benzoate | HCID 11952920 | — |
反応手順
To a slight suspension of 4-methyl-3-(trifluoromethyl)benzoic acid (2.18 g, 10.7 mmol, ABCR) in ethanol (30 ml) was added concentrated sulphuric acid specific gravity 1.84 (0.5 ml, 9.38 mmol). The resulting solution was heated to reflux overnight under nitrogen. The solution was diluted with DCM (100 ml) and then water (100 ml). The phases were separated and the organic extract washed with saturated aqueous sodium hydrogen carbonate (50 ml), dried (MgSO4), filtered and the solvent removed in vacuo to give the title compound as a mobile pale yellow oil (2.27 g); LCMS: (System 4) MH+=233, tRET=3.29 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08399436B2 |
| 出典データセット | uspto-grants-2013_03 |
| ORD ID | ord-33fc9be909894b4aa99015fc66305992 |
| 出典メモ | uspto-grants-2013_03 |