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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 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 4-Methyl-3-(trifluoromethyl)benzoic acid | HCID 2775592 | — |
| 生成物 | Ethyl 4-methyl-3-(trifluoromethyl)benzoate | HCID 11952920 | — |
反応手順
A solution of commercially available 4-methyl-3-trifluoromethylbenzoic acid (24.5 g, 120 mmol) and conc. sulfuric acid (6.5 ml) in dry ethanol (245 ml) is refluxed for 23 h. After reaching room temperature the solvent is evaporated and the residue is neutralized by addition of saturated aqueous NaHCO3 solution. The mixture is extracted with ethyl acetate (3×40 ml). The organic extracts are combined, dried over Na2SO4 and evaporated to dryness to afford a pale yellow oil: HPLC: tR=7.15 min (purity: >96%, gradient A), ESI-MS: 233.3 [MH]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08552002B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-12b25178549c4aba98b40378a1cdd289 |
| 出典メモ | uspto-grants-2013_10 |