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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 | Ethanol | HCID 702 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one | HCID 11401769 | — |
反応手順
At ambient temperature, 35 g (159.6 mmol) of 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one are dissolved in a mixture of 525 mL of ethanol and 175 mL of ethyl acetate. There are then added 7 g (20% by weight) of palladium-on-carbon 10% and hydrogenation is carried out at 65° C. and 3.5 bars for 22 hours. The catalyst is filtered off over Celite; rinsing with a mixture of ethanol/ethyl acetate and evaporation to dryness are carried out to yield the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08076325B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-79e09f955b0c4e83b82d3cfe11708c5c |
| 出典メモ | uspto-grants-2011_12 |