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Ethanol → Ethyl 3,4-dichlorophenylacetate
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 | 3,4-Dichlorophenylacetic acid | HCID 79874 | — |
| 生成物 | Ethyl 3,4-dichlorophenylacetate | HCID 2737422 | 82.5% |
反応手順
A solution of (3,4-dichloro-phenyl)-acetic acid (10.0 g, 0.048 mol) in ethanol (50 mL) was treated with a catalytic amount of sulfuric acid. The reaction mixture was refluxed for 7 h. The reaction was concentrated in vacuo, diluted with diethyl ether, and poured into water. The ether layer was washed with a saturated aqueous sodium bicarbonate solution and water. The organics were then dried over sodium sulfate, filtered, and concentrated in vacuo. Vacuum distillation (bath temperature: 175° C.; head temperature: 125° C.) afforded (3,4-dichloro-phenyl)-acetic acid ethyl ester (9.38 g, 82.5%) as a clear oil: EI-HRMS m/e calcd for C10H10Cl2O2 (M+) 232.0058, found 232.0066.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06528543B1 |
| 出典データセット | uspto-grants-2003_03 |
| ORD ID | ord-65ffea5f22d74b8181f96cbe5c9fbb5f |
| 出典メモ | uspto-grants-2003_03 |