化工社化工社 化学情報印刷レポート · 研究参考用
1-Chloro-4-nitrobenzene → 1-(4-Nitrophenyl)-1,4-diazepane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Chloro-4-nitrobenzene | HCID 7474 | — |
| 反応物 | Hexahydro-1,4-diazepine | HCID 68163 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 1-(4-Nitrophenyl)-1,4-diazepane | HCID 5055950 | 42% |
反応手順
A solution of homopiperazine (11.4 g, 114 mmol) in 1-butanol (40 mL) was added to a refluxing solution of 1-chloro-4-nitrobenzene (6.0 g, 38 mmol) in 1-butanol (40 mL) over 15 minutes. The mixture was maintained at reflux for 24 hours then cooled to room temperature and extracted with 2N hydrochloric acid. The aqueous layer was basified with potassium carbonate and extracted with ethyl acetate. The organic layer was dried over sodium sulfate and concentrated to afford 1-(4-nitro-phenyl)-[1,4]diazepane (3.5 g, 42%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524705B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-4c60e14d135f433dad7b2bd9ef175647 |
| 出典メモ | uspto-grants-2013_09 |