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1,3-Dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one → 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one | HCID 1482373 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one | HCID 11401769 | — |
反応手順
A suspension of 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one (21.9 g, 0.1 mol) and 10% palladium/charcoal (1.5 g) in glacial acetic acid (200 ml) is hydrogenated at 50° C. under a hydrogen pressure of 5 bar. After the catalyst has been filtered off the solvent is evaporated in vacuo and the residue is taken up in methylene chloride. After extraction with sodium bicarbonate solution and washing with water, the product is dried over magnesium sulphate, concentrated by evaporation and purified over silica gel with methylene chloride and then with increasing amounts of methanol (up to 10%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04737495 |
| 出典データセット | uspto-grants-1988_04 |
| ORD ID | ord-04c6be61b72646a7b422c1fdb6bb4583 |
| 出典メモ | uspto-grants-1988_04 |