関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 1-Bromooctane | HCID 8140 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,7-Dibromofluorene | HCID 140073 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,7-Dibromo-9,9-di-n-octylfluorene | HCID 5215321 | 79% |
反応手順
2,7-di bromo fluorene (25 g, 77 mmol), octylbromide (44.7 g, 0.596 mols), sodium hydroxide (37.5 g, 0.937 mols), and tetrabutyl ammonium bromide (0.5 g, 1.55 mmol) were dissolved in dimethyl sulfoxide (75 ml)-water (37.5 ml) mixed solvent. It was kept warm at 80° C. for 6 hours. After cooling, toluene (100 ml) and water (100 ml) were added, and the organic layer was partitioned. The organic layer is washed with water, 3% hydrochloric acid, and water, and then dehydrated with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the crude product was purified by silica-gel chromatography, and 2,7-dibromo-9,9-dioctylfluorene was obtained. (Amount: 26.85 g, yield: 79%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07701129B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-aa7caae9fe6a44939a101baec01465c4 |
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| 出典メモ | uspto-grants-2010_04 |
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