関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,7-Dibromofluorene | HCID 140073 | — |
| 反応物 | 9-(10-Bromodecyl)-9H-carbazole | HCID 21976310 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9,9-Bis(N-carbazolyl-decyl)-2,7-dibromofluorene | HCID 21044128 | 34.1% |
反応手順
To a mixture of 5.2 g (16 mmol) 2,7-dibromofluorene in 300 mL THF was added 1.3 g (41 mmol) sodium hydride (75%) in several portions. A mixture of 15 g (39 mol) N-(10-bromodecyl)-carbazole (8) in 100 mL THF was added dropwisely at 70° C. and the mixture was refluxed for 48 h. After cooling, the solid was filtered and the filtrate was concentrated and dilute with water and extracted with CH2Cl2. The organic layer was collected and washed with brine and dried with anhydrous MgSO4. The crude product was further purified by silica column chromography to give 5.1 g (yield 34%, mp 94˜96° C.) title product. 1H NMR (CDCl3), δ (ppm): 8.10 (4H, d), 7.38˜7.48 (14 H, m), 7.23 (4H, t), 4.27 (4H, t), 0.88˜1.86 (36H, m). Anal. Calcd: C, 73.22; H, 6.68; N, 3.00. Found: C, 72.58; H, 6.59; N, 2.73.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07220819B2 |
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| 出典データセット | uspto-grants-2007_05 |
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| ORD ID | ord-2d60f307539c4c0c9c21aec458cb0ea1 |
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| 出典メモ | uspto-grants-2007_05 |
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