関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Butyl iodide | HCID 10962 | — |
| 反応物 | 2-Iodo-9H-fluorene | HCID 224094 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9,9-dibutyl-2-iodo-9H-fluorene | HCID 23072853 | — |
反応手順
20 parts of 2-iodofluorene was dissolved in a mixed solution of 114 parts of dimethyl sulfoxide (DMSO) and 23 parts of tetrahydrofuran (THF), and the thus obtained mixture was then stirred at 25° C. for 10 minutes. Thereafter, while stirring, 8.6 parts of potassium-tert-butoxide was added to the mixture. Twenty minutes later, 14.6 parts of butyl iodide was added to the mixture, and further twenty minutes later, 8.6 parts of potassium-tert-butoxide was added thereto. Further, twenty minutes later, 14.6 parts of butyl iodide was added thereto, and the obtained mixture was then stirred at 25° C. for 2 hours. After completion of the stirring, THF was distilled away from the reaction solution, and it was then extracted with toluene-water. The toluene phase was dried over magnesium sulfate, and toluene was then distilled away, thereby obtaining a brown tarry solid. This brown tarry solid was separated and purified by column chromatography (hexane-ethyl acetate) to obtain 25 parts of 9,9-dibutyl-2-iodofluorene in the form of a colorless crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08735720B2 |
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| 出典データセット | uspto-grants-2014_05 |
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| ORD ID | ord-2f03f86e82c54fe2b75ef364dc7adb49 |
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| 出典メモ | uspto-grants-2014_05 |
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