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trans-3-(3-Pyridyl)acrylic acid → (E)-N-(3-hydroxyphenethyl)-3-(3-pyridyl)-2-propenoic acid amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | trans-3-(3-Pyridyl)acrylic acid | HCID 776396 | — |
| 反応物 | 3-(2-Aminoethyl)phenol hydrobromide | HCID 22717856 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Pivaloyl chloride | HCID 62493 | — |
| 生成物 | (E)-N-(3-hydroxyphenethyl)-3-(3-pyridyl)-2-propenoic acid amide | HCID 23067308 | 78.1% |
反応手順
To a solution of trans-3-(3-pyridyl)acrylic acid (179 g) in dichloromethane (4.8 L), triethylamine (584 ml) and pivaloyl chloride (148 ml) were sequentially added under ice-cooling and stirring and stirred for 15 minutes. Subsequently, 3-hydroxyphenethylamine hydrobromide (263 g) was added at the same temperature and stirred for 2 hours. After the solvent was distilled out under reduced pressure, water was added to the residue and the precipitated crystal was filtered, washed with water and recrystallized in ethanol to yield the titled compound (251.4 g, 78%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06313153B1 |
| 出典データセット | uspto-grants-2001_11 |
| ORD ID | ord-30bbc6d9862246738c5adb93bfdae549 |
| 出典メモ | uspto-grants-2001_11 |