関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Bromo-3,4,5-trifluorobenzene | HCID 611409 | — |
| 反応物 | p-Formylphenylboric acid | HCID 21940015 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3',4',5'-Trifluoro-[1,1'-biphenyl]-4-carbaldehyde | HCID 61239877 | 96.9% |
反応手順
In a nitrogen atmosphere, a solution prepared by mixing 15.00 g of 3,4,5-trifluorobromobenzene, 0.25 g of tetrakis-triphenylphosphine palladium, 30 mL of an aqueous potassium carbonate solution (2 mol/L), and 75 mL of THF was heated to 60° C., and 10.71 g of 4-formylphenylboric acid was added to the solution over 20 minutes. After the resultant mixture was stirred at 60° C. for 3 hours, the mixture was allowed to cool, and an organic layer was separated by adding hexane. The organic layer was washed with saturated brine and dried by adding sodium sulfate, and then the solvent was distilled off under reduced pressure. As a result of purification by silica gel column chromatography, 14.77 g of 4-(3,4,5-trifluorophenyl)benzaldehyde was yielded.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08916718B2 |
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| 出典データセット | uspto-grants-2014_12 |
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| ORD ID | ord-1f4bff464cbe48f4820367ccdde28900 |
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| 出典メモ | uspto-grants-2014_12 |
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