参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 反应物 | Carbonic acid sodium salt (1:2) | HCID 10340 | — |
| 反应物 | 1-溴-3-碘苯 | HCID 11561 | — |
| 反应物 | 5-甲醛基呋喃-2-硼酸 | HCID 2734355 | — |
| 催化剂 | HCID 178418397 | HCID 178418397 | — |
| 溶剂 | 乙二醇二甲醚 | HCID 8071 | — |
| 产物 | 5-(3-溴苯基)呋喃-2-甲醛 | HCID 840517 | 25.9% |
反应步骤
5-Formyl-2-furanboronic acid (676 mg, 4.8 mmol) and 3-bromoiodobenzene (1132 mg, 4 mmol) were dissolved in 1,2-dimethoxyethane (30 mL), tetrakis(triphenylphosphine)palladium (228 mg, 0.2 mmol) was added thereto, 2 mol/L sodium carbonate (9.6 mL) was further added thereto, and the mixture was heated to reflux for 2 hours while stirring. After the reaction was completed water (20 mL) was added thereto, and extraction with ethyl acetate (20 mL×2) was carried out. The organic layer was washed with saturated brine, water was removed using anhydrous sodium sulfate, the solvent was then removed by evaporation under reduced pressure, and the residue was subjected to silica gel column chromatography using ethyl acetate/hexane (3/7 (volume ratio)) as an eluent, to give 5-(3-bromophenyl)furan-2-carbaldehyde in a yield of 306 mg (yield 25.9%).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US08476449B2 |
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| 来源数据集 | uspto-grants-2013_07 |
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| ORD ID | ord-5e7c749d4a9446d4a9a263f8c69dd32d |
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| 来源说明 | uspto-grants-2013_07 |
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