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Phosphorus oxychloride → Benzaldehyde, 4-[[2-(acetyloxy)ethyl]ethylamino]-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Ethanol, 2-(ethylphenylamino)-, 1-acetate | HCID 113382 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benzaldehyde, 4-[[2-(acetyloxy)ethyl]ethylamino]- | HCID 11458991 | 84.2% |
反応手順
After adding 55.8 g of ice-cooled phosphoryl chloride to 26.6 g of dimethylformamide, a solution of 63.0 g of the 2-(N-ethylanilino)ethyl acetate in 40 ml of dimethylformamide was slowly added at room temperature, this was caused to react for 6 hours at room temperature while stirring, and then poured into an aqueous solution of 150 g of sodium acetate under ice cooling. An organic layer was extracted with ethyl acetate and the solvent was boiled off under reduced pressure. This was refined by silica gel column chromatography to yield 60.2 g of 2-(ethyl(4-formylphenyl)amino)ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06383714B1 |
| 出典データセット | uspto-grants-2002_05 |
| ORD ID | ord-cd1897f09e154f11a129d2603cfaff4e |
| 出典メモ | uspto-grants-2002_05 |