化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dibromoethane → 1-(2-Bromoethyl)-2a,3,4,5-tetrahydrobenz[cd]indole-2(1H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2a,3,4,5-Tetrahydrobenzo[cd]indol-2(1H)-one | HCID 599375 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(2-Bromoethyl)-2a,3,4,5-tetrahydrobenz[cd]indole-2(1H)-one | HCID 22629573 | 34% |
反応手順
2a,3,4,5-Tetrahydrobenz[cd]indole-2(1H) -one (3.46 g, 20mmol) was dissolved in anhydrous N,N-dimethylformamide (20 ml). Thereto was added sodium hydride (0.8 g, 20 mmol), and the resulting solution was stirred at room temperature for 1 hour. The reaction solution was mixed with 1,2-dibromoethane (10 ml, 115 mmol) and again stirred for 1 hour. The reaction solution was extracted by adding 100 ml of ethyl acetate and 100 ml of water, and the resulting ethyl acetate layer was separated, washed with water and dried with anhydrous sodium sulfate. Then the compound obtained by the evaporation of the solvent under a reduced pressure was crystallized from a dimethylformamide-water mixture to obtain 1.9 g of the title compound (34% in yield).
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-161e0de06b4448e39e039f9cdf33adef |
| 出典メモ | uspto-grants-2002_03 |