化工社化工社 化学情報印刷レポート · 研究参考用
Water → 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,3,4,5-Tetrahydro-1H-benzo(d)azepine | HCID 1400243 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 19375487 | 95% |
反応手順
A solution of acetic anhydride (6.37 g, 0.062 mol) in dichloromethane (50 ml) was added dropwise to a stirred solution of 2,3,4,5-tetrahydro-1H-3-benzazepine (8.35 g, 0.057 mol) and triethylamine (8.7 ml) in dichloromethane (50 ml) at 0° C. under argon. After stirring at room temperature for 18 h, water (80 ml) was added and the organic layer separated. The organic layer was washed with 0.5 M hydrochloric acid (50 ml), saturated sodium bicarbonate solution (50 ml), water (50 ml) and then dried (Na2SO4). Evaporation of the solvent in vacuo gave the title compound (10.24 g, 95%) as a yellow oil which solidified on standing.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06605607B1 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-cfd8b7ddc4d7472d808255188e65c0a5 |
| 出典メモ | uspto-grants-2003_08 |