化工社化工社 化学情報印刷レポート · 研究参考用
Water → 3-(4-Chlorobut-1-yl)-3-azabicyclo[3.1.0]hexane-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Azabicyclo[3.1.0]hexane-2,4-dione | HCID 3720053 | — |
| 反応物 | 1-Chloro-4-iodooctane | HCID 23289978 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(4-Chlorobut-1-yl)-3-azabicyclo[3.1.0]hexane-2,4-dione | HCID 23289986 | — |
反応手順
Sodium hydride (0.11 g, 60% dispersion in oil) was added to a stirred solution of 3-azabicyclo[3.1.0]hexane-2,4-dione (0.5 g) and 1-chloro-4-iodooctane (0.98 g) in dry dimethylformamide (50 ml) under a nitrogen atmosphere at room temperature. The resulting mixture was stirred for 48 hours and water (50 ml) was then added dropwise. The aqueous mixture was extracted with dichloromethane (2×200 ml) and the combined organic extracts were then washed with water (2×400 ml), dried (MgSO4) and evaporated in vacuo to give an oil. The oil was purified by chromatography on silica (80 g) using 1:1 ethyl acetate/hexane as eluant to give the title compound as a colourless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06130241 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-f61baab36b774972a71ac6203a4fc40d |
| 出典メモ | uspto-grants-2000_10 |