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o-Phenetidine → N-(2-Ethoxyphenyl)-2-methylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | o-Phenetidine | HCID 7203 | — |
| 反応物 | 2-Methylbenzoic acid | HCID 8373 | — |
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | N-(2-Ethoxyphenyl)-2-methylbenzamide | HCID 576828 | 94.5% |
反応手順
A 13.6 g (0.1 mol) portion of o-methylbenzoic acid and 13.7 g of o-ethoxyaniline were dissolved in 200 ml of acetone. A 4.7 g (0.033 mol) amount of phosphorus pentoxide was gradually added to the prepared solution at 30° - 40° C. After the addition, the reaction mixture was refluxed for 3 hours with stirring. The acetone was removed and the residual product was poured into water and was extracted with toluene. The toluene layer was dried over anhydrous sodium sulfate and the toluene was removed to obtain 24.1 g (94.5%) of a clear pink liquid, having a boiling point of 148° C/0.04 mm Hg and nD20 of 1.5929.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03985804 |
| 出典データセット | uspto-grants-1976_10 |
| ORD ID | ord-2dacb707b5fd4549a1c468081797601d |
| 出典メモ | uspto-grants-1976_10 |