関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 4-Bromo-2-methylbenzoic acid | HCID 99570 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3-Formylphenyl dihydrogen borate | HCID 21987105 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl 4-(3-formylphenyl)benzoate | HCID 4321386 | — |
反応手順
A solution of tetrakis(triphenylphosphine)palladium (297 mg) was added to a solution of 3-formylphenylboric acid (3.00 g) and methyl 4-bromobenzoic acid (4.30 g) in a mixture of toluene (30 ml), ethanol (50 ml) and saturated aqueous sodium hydrogencarbonate solution (30 ml) at ambient temperature. The mixture was heated at reflux for 2 hours at 100° C. The reaction mixture was partitioned between ethyl acetate and water and the layers were separated. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was crystallized from diisopropyl ether to afford the title compound (3.37 g) as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06528525B1 |
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| 出典データセット | uspto-grants-2003_03 |
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| ORD ID | ord-1bda2d917f2f471eb1211d82bf09e522 |
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| 出典メモ | uspto-grants-2003_03 |
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