참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Bromooctane | HCID 8140 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2,7-Dibromofluorene | HCID 140073 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,7-Dibromo-9,9-di-n-octylfluorene | HCID 5215321 | 150.4% |
반응 단계
To a solution of 28.5 g (88 mmol) 2,7-dibromofluorene in 800 mL THF was added 8.8 g (220 mmol) sodium hydride (60%) in several portions at room temperature. The mixture was heated at 60° C. and 43 g (220 mmol) bromooctane in 200 mL THF was added dropwisely into the mixture and refluxed overnight. The mixture was concentrated and diluted with water, and then extracted with diethyl ether. After washing with brine, the ether solution was dried over anhydrous MgSO4 and the ether was then removed by evaporation. This crude solid was purified by a silica chromography with hexane and recrystallized from ethanol to give white solid (36.3 g, yield 75.3%, mp. 52˜54° C.). 1H NMR (500 MHz, CDCl3), δ (ppm): 7.51 (2H, d), 7.44 (2H, d), 7.41 (2H, s), 1.89 (4H, m), 1.02˜1.20 (20H, m), 0.81 (6H, t), 0.56 (4H, m).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07098295B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-da03422107184f23b2816271e7ba8577 |
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| 출처 메모 | uspto-grants-2006_08 |
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