関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Dimethyl 4,4'-biphenyldicarboxylate | HCID 13099 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 生成物 | 4,4-Bis(Hydroxymethyl)Biphenyl | HCID 68743501 | 93% |
反応手順
In a 1000 ml three-necked flask, fitted with an efficient condenser, a thermometer and a dropping funnel, is placed a suspension of 6,2 g (0.144 mol) LiAlH4 in 80 ml dry THF under an inert atmosphere. A solution of 30 g (0.122 mol) dimethyl 4,4'-biphenyldicarboxylate in 250 ml dry THF is added dropwise over a period of 30 minutes. The mixture is refluxed with stirring for 1 hour. The mixture is cooled to -20° C. and 80 ml of H2O is added dropwise, followed by slow addition of 80 ml of 20% H2SO4 (aq.). The THF is evaporated under reduced pressure to give a suspension of colourless product in aqueous acid. The product is filtered and washed with H2O. After recrystallisation from aceton, white crystals are obtained. Yield: 93%; melting point: 187.3° C.-188.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05763539 |
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| 出典データセット | uspto-grants-1998_06 |
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| ORD ID | ord-63b2289b48a74ce58fc15c0884e38cf7 |
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| 出典メモ | uspto-grants-1998_06 |
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