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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
55.8 g of phosphoryl chloride cooled with ice was added to 26.6 g of N,N-dimethyl formamide. To this, a solution of 63.0 g of the 2-(N-ethylanilino)ethyl acetate and 40 ml of N,N-dimethyl formamide was added slowly at room temperature. The resulting solution was stirred for 6 hours at room temperature for reaction, and then was poured in an aqueous solution of 150 g of sodium acetate that was being cooled with ice water. The organic layer was extracted with ethyl acetate. The solvent was then distilled off under reduced pressure and purified by chromatography on silica, to obtain 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 | US06355396B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-28c3ba2832d7496783de23f90c23950f |
| 出典メモ | uspto-grants-2002_03 |