참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2,4,5-Triphenylimidazole | HCID 10232 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1,8-Dibromooctane | HCID 78310 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(8-Bromooctyl)-2,4,5-triphenylimidazole | HCID 22916437 | 50% |
반응 단계
2,4,5-Triphenylimidazole (5 g) was added to a suspension of sodium hydride (1.0 g) (50% dispersion in oil, washed with hexane) in dry dimethylformamide (80 ml) under nitrogen. The reaction was stirred at 45° C. for 1 h, cooled and added, over 1 h to a solution of 1,8-dibromo-octane (30 g) in dry dimethylformamide (100 ml) under nitrogen. The reaction was stirred at room temperature for 24 h, water was carefully added and the solvent was removed in vacuo. The residue was dissolved in ethyl acetate (500 ml), washed with water (250 ml), 2N aqueous hydrochloric acid (250 ml), saturated sodium chloride solution (250 ml), dried over anhydrous magnesium sulphate and evaporated to dryness in vacuo. Distillation to remove 1,8-dibromooctane and chromatography on silica gel eluted with dichloromethane gave 1-(8-bromooctyl)-2,4,5-triphenylimidazole (4.1 g, 50%) as an oil; NMR d (CDCl3) 0.9-1.7 (12H, m, 6×CH2), 3.3 (2H, t, BrCH2), 3.9 (2H, t, N--CH2), 7.1-7.7(15H, m, 3×Ph) ppm.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05648373 |
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| 출처 데이터셋 | uspto-grants-1997_07 |
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| ORD ID | ord-711ec5d42d0d4235916d1f906fd9f1f0 |
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| 출처 메모 | uspto-grants-1997_07 |
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