関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Benzhydrylpyridine | HCID 77252 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Acetonitrile methanol | HCID 21959252 | — |
| 生成物 | 4-(Diphenylmethyl)piperidine hydrochloride | HCID 23004093 | — |
反応手順
A mixture of 62.69 g (0.256 mole) of diphenyl-4-pyridylmethane and 6.4 g of 10% palladium on carbon (0.0060 mole) in 300 ml of glacial acetic acid and under an atmosphere of hydrogen (44 psi) was shaken on a Parr apparatus at 865° for 4 days. The reaction mixture was filtered, and the solvent was removed in vacuo from the filtrate. The residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give a solid. This was dissolved in a mixture of methanol-acetonitrile, and excess ethereal hydrogen chloride was added. A precipitate was collected to give 59.13 g (80.3%) of slightly impure title compound as a white, crystalline solid, m.p. 273°-274° C. Part of this was recrystallized from methanol-ether to give an analytically pure sample, m.p. 275.5°-277° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04950674 |
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| 出典データセット | uspto-grants-1990_08 |
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| ORD ID | ord-fab04107275b4890aeb9f104e17555f5 |
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| 出典メモ | uspto-grants-1990_08 |
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