関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Dibromopropane | HCID 8001 | — |
| 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 | 2a-(3-Bromopropyl)-2a, 3,4,5-tetrahydrobenz[cd]indole-2(1H)-one | HCID 15542633 | 8.8% |
反応手順
2a, 3,4,5-Tetrahydrobenz [cd]indole-2(1H) -one (1.0 g, 5.8 mmol) was dissolved in anhydrous N,N-dimethylformamide (40 ml). Thereto was added sodium hydride (230 mg, 5.8 mmol), and the resulting solution was stirred at 60° C. for 1 hour. The reaction solution was mixed with 1,3-dibromopropane (1.8 ml, 17 mmol) and again stirred for 2 hours. The solvent was evaporated under a reduced pressure, and the thus obtained residue was mixed with ethyl acetate and water. The reaction product was extracted with ethyl acetate, washed with saturated brine and dried with anhydrous sodium sulfate. Then the compound obtained by the evaporation of the solvent under a reduced pressure was separated and purified by a silica gel column chromatography to obtain 150 mg of the title compound (0.51 mmol, 8.8% in yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06355642B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-df257ab28db0484287d8fde9c306582f |
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| 出典メモ | uspto-grants-2002_03 |
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