化工社化工社 化学情報印刷レポート · 研究参考用
Water → 2-Ethyl-1-(4-methoxyphenyl)butan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Ethylbutyric acid | HCID 6915 | — |
| 反応物 | Anisole | HCID 7519 | — |
| 反応物 | Dysprosium(III) trifluoromethanesulfonate | HCID 9938788 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Ethyl-1-(4-methoxyphenyl)butan-1-one | HCID 245508 | 44% |
反応手順
Dysprosium (III) trifluoromethanesulfonate (3.66 g as a wet solid), anisole (1.08 g) and 2-ethylbutanoic acid (1.16 g) were refluxed together in 125 mL toluene with azeotropic removal of the lower water layer (Dean-Stark apparatus). After 48 hours, the mixture was cooled and extracted with 3×25 mL water, then by 2×25 mL saturated sodium bicarbonate solution. The organic layer was dried using anhydrous sodium sulfate, filtered, then concentrated down in vacuo to give para-methoxy-2-ethylbutyrophenone (0.90 g, 44% yield) as an amber-colored oil, which was practically pure by 1H NMR analysis. Removal of water from the three water extracts recovered 3.54 g as a damp, off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06362375B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-a84ca71e99714676b1d7c6d5d5c20d10 |
| 出典メモ | uspto-grants-2002_03 |