参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 正己烷 | HCID 8058 | — |
| 反应物 | 2-溴-6-甲基吡啶 | HCID 79205 | — |
| 反应物 | 4,5-二甲基-2-糠醛 | HCID 643406 | — |
| 反应物 | 正丁基锂 | HCID 178418339 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 溶剂 | 四氢呋喃 | HCID 8028 | — |
| 产物 | HCID 23078353 | HCID 23078353 | 80% |
反应步骤
2-Bromo-6-picoline (1.5 g) was dissolved in tetrahydrofuran (40 ml) under an argon atmosphere to prepare a solution. A 1.6 M hexane solution (5.6 ml) of n-butyllithium was added dropwise to the solution at −78° C., and the mixture was then stirred at −78° C. for 30 min. A solution of 4,5-dimethylfurfural (1 g) in tetrahydrofuran (20 ml) was added dropwise thereto, and the temperature of the mixture was raised to room temperature while stirring. Water was added to the reaction solution to stop the reaction, and the solvent was removed by distillation under the reduced pressure. Water was added to the residue, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using hexane-acetone to give (4,5-dimethylfuran-2-yl)-(6-methyl-pyridin-2-yl)-methanol (1.4 g, yield 74%).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US07560558B2 |
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| 来源数据集 | uspto-grants-2009_07 |
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| ORD ID | ord-184fa0e40e7b4fb6846e0d92c287f54f |
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| 来源说明 | uspto-grants-2009_07 |
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