関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Stilbene | HCID 11502 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Dibenzyl | HCID 7647 | 92.5% |
反応手順
To a dry, nitrogen-filled 250 ml single-necked round-bottom flask fitted with a nitrogen inlet and magnetic stirring bar was added 11.8 g (65.5 mmol) of stilbene, 11 g (240 mmol) formic acid, 5 g of 10% Pd on activated carbon (4.7 mmol Pd), 60 ml of absolute ethanol and 100 ml of dry benzene. The reaction vessel was placed in a sonicator so that the liquid level inside the flask matched that of the bath water and in the location that produced the maximum cavitation in the flask. After 1 h the flask was removed and the contents filtered. The solid was washed with chloroform and the combined filtrates concentrated on a rotary evaporator. The residual soild was recrystallized (ethanol-pentane) to give 11.03g (92.5% yield) of bibenzyl mp 51°-51.5° (lit 52.5) (8).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04466870 |
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| 出典データセット | uspto-grants-1984_08 |
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| ORD ID | ord-40f363345bb14156a5e6e204c259faf9 |
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| 出典メモ | uspto-grants-1984_08 |
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