化工社化工社 化学情報印刷レポート · 研究参考用
Acetyl chloride → 1-(8-Nitro-2,3,4,5-tetrahydro-benzo[b]azepin-1-yl)-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 8-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine | HCID 46864071 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(8-Nitro-2,3,4,5-tetrahydro-benzo[b]azepin-1-yl)-ethanone | HCID 57470257 | 81.6% |
反応手順
Acetyl chloride (1 g, 13 mmol) was added dropwise to a mixture of 8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.3 g, 6.8 mmol) and NaHCO3 (1 g, 12 mmol) in CH2Cl2 (50 mL). After stirring for 1 h, the mixture was filtered and the filtrate was concentrated. The residue was dissolved in CH2Cl2, washed with brine, dried over Na2SO4 and concentrated. The residue was purified by column chromatography to give 1-(8-nitro-2,3,4,5-tetrahydro-benzo[b]azepin-1-yl)-ethanone as a yellow solid (1.3 g, 80%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08741925B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-500a13aed2c34aa591c5d710fad33eae |
| 出典メモ | uspto-grants-2014_06 |