関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Thiophene | HCID 8030 | — |
| 反応物 | 1-Bromohexane | HCID 8101 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 2-Hexylthiophene | HCID 87793 | 75% |
反応手順
To a cooled (−70° C.) mixture of thiophene (17.6 g, 0.21 mol) in anhydrous THF (100 mL) was added dropwise a solution of n-BuLi (137.5 ml, 1.6 M, 0.22 mol) in hexane. After stirring for 1 hour at 0° C., the mixture was cooled to −40° C. followed by addition of 1-hexylbromide (0.22 mol). The mixture was slowly heated to r.t. Water (250 mL) was added and the mixture was extracted with diethylether (3×150 mL). The combined organic fractions were dried over MgSO4 and concentrated in vacuo. The product was purified by means of vacuum distillation. This product was prepared according to the general procedure and obtained as a colourless oil (26.5 g, 75%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08367717B2 |
|---|
| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-b440b94418404c5e87dfa632619d5aab |
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| 出典メモ | uspto-grants-2013_02 |
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