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Hydrochloric Acid → 4-(Ethyl(2-hydroxyethyl)amino)benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-(N-Ethyl-4-formylanilino)ethyl benzoate | HCID 104564 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(Ethyl(2-hydroxyethyl)amino)benzaldehyde | HCID 639857 | 51% |
反応手順
4-Formyl-N-ethyl-N-(2-benzoyloxyethyl)aniline (16 g, 51 mmol) was added to a stirring suspension of potassium carbonate (9 g, 65 mmol) in methanol (150 mL) and water (50 mL). Stirring was continued at room temperature for 4 hours followed by addition of 1 molar hydrochloric acid (250 mL) and extraction into diethyl ether (3×100 mL). The combined ether layers were washed with saturated sodium bicarbonate (200 mL), water (200 mL), saturated sodium chloride (200 mL), dried over magnesium sulfate and the solvent was removed under reduced pressure. The crude product was purified using a silica gel chromatography column eluting with 50% ethyl acetate in hexane which gave the compound as a clear yellow oil (5 g, 51% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05212269 |
| 出典データセット | uspto-grants-1993_05 |
| ORD ID | ord-7d992ac09afe4dee9848fa024a9ee2ae |
| 出典メモ | uspto-grants-1993_05 |