化工社化工社 化学情報印刷レポート · 研究参考用
Methyl iodide → Benz[cd]indol-2(1H)-one, 1-methyl-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | benz(cd)indol-2(1H)-one | HCID 67222 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benz[cd]indol-2(1H)-one, 1-methyl- | HCID 121175 | — |
反応手順
Benz[cd]indole-2(1H)-one (5.1 g, 30 mmol) was dissolved in anhydrous N,N-dimethylformamide (100 ml). Thereto was added sodium hydride (60% content, 1.2 g, 30 mmol), and the resulting solution was stirred for 20 minutes in an ice bath. The reaction solution was mixed with methyl iodide (2.6 ml, 42 mmol) and again stirred at a room temperature for 1 hour. The reaction solution was mixed with ethyl acetate (300 ml) and water (200 ml), and the reaction product was extracted with ethyl acetate. The ethyl acetate layer was separated, washed with water and then dried with anhydrous sodium sulfate. By evaporating ethyl acetate under a reduced pressure, 4.7 g (26 mmol, 74% in yield) of the title compound was obtained as yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06355642B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-33e2ed34f1e1450dbb0cd6f36ec282a8 |
| 出典メモ | uspto-grants-2002_03 |