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Potassium Carbonate → 7-Methoxy-2,3,4,5-tetrahydro-1H-2-benzazepin-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-Methoxy-alpha-tetralone | HCID 14112 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 7-Methoxy-2,3,4,5-tetrahydro-1H-2-benzazepin-1-one | HCID 4230609 | — |
反応手順
Sodium azide (0.37 g) was slowly added in portions to a stirring ice-cold suspension of 6-methoxy-3,4-dihydro-2H-naphthalen-1-one in 10 mL of concentrated hydrochloric acid. The mixture was allowed to slowly warm to room temperature and stirred for 20 h. The mixture was poured onto ice and carefully neutralized with solid potassium carbonate. The resulting mixture was extracted with two 50 mL aliquots of dichloromethane. The organic material was dried over sodium sulfate and the solvent was evaporated. Chromatography (ethyl acetate) gave 0.45 g of 7-methoxy-2,3,4,5-tetrahydrobenzo[c]azepine-1-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084154B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-141213c897394fb3aee98326e828dc45 |
| 出典メモ | uspto-grants-2006_08 |