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Ammonia → 8-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Potassium Nitrate | HCID 24434 | — |
| 反応物 | 2,3,4,5-tetrahydro-1H-1-benzazepine | HCID 576503 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 8-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine | HCID 46864071 | 52% |
反応手順
At −10° C., 2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.9 g, 13 mmol) was added dropwise to a solution of KNO3 (3 g, 30 mmol) in H2SO4 (50 mL). The mixture was stirred for 40 min, poured over crushed ice, basified with aq. ammonia to pH 13, and extracted with EtOAc. The combined organic phases were washed with brine, dried over Na2SO4 and concentrated to give 8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine as a black solid (1.3 g, 51%), which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829204B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-4408e440c14949c580c69743d4cbf49b |
| 出典メモ | uspto-grants-2014_09 |