関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Dimethyl 4,4'-biphenyldicarboxylate | HCID 13099 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | [1,1'-Biphenyl]-4,4'-dicarboxaldehyde | HCID 6200 | 86.1% |
反応手順
Next, 27.1 g (0.10 mole) of dimethyl 4,4′-biphenyldicarboxylate and 133.4 g of THF were introduced to a 2000-ml four-necked reaction vessel. To this solution was added the reagent solution prepared above in drops at 5° C. or below. After the dropwise addition, stirring was continued at 15° C. for 4.5 hours. Upon completion of the reaction, extraction was performed by adding in drops 622.2 g of methylene chloride and 411.2 g of water. The methylene chloride layer obtained was concentrated until dryness under reduced pressure. The residue was dissolved in acetone by adding 303.2 g of acetone in drops and then 1600.3 g of water was added in drops at 20° C. Thereafter, the mixture was stirred day and night at 5° C. and a solid was recovered by filtration. The solid thus obtained was washed with acetone and dried under reduced pressure to give 18.1 g of 4,4′-biphenyldicarboxaldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07582364B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-25c872cf8d544280ace618887109e235 |
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| 出典メモ | uspto-grants-2009_09 |
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