関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butanal | HCID 261 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 1-(4-Methoxyphenyl)-piperazine, dihydrochloride | HCID 2723700 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-Butyl-4-(4-methoxyphenyl)piperazine dihydrochloride | HCID 20519334 | 81% |
反応手順
A mixture of 13.2 parts of 1-(4-methoxyphenyl)piperazine dihydrochloride, 5.1 parts of 1-butanal, 9 parts of sodium acetate and 80 parts of methanol is hydrogenated at normal pressure and at room temperature with 1 part of palladium-on-charcoal catalyst. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and the filtrate is evaporated. Water is added to the residue and the product is precipitated. It is filtered off, washed with water and converted into the hydrochloride salt in ethanol and 2-propanol. Upon the addition of 2,2'-oxybispropane, the salt is precipitated. It is filtered off and crystallized from a mixture of ethanol and 2,2'-oxybispropane, yielding 13.1 parts (81%) of 1-butyl-4-(4-methoxyphenyl)piperazine dihydrochloride; mp. 214.2° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04358449 |
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| 出典データセット | uspto-grants-1982_11 |
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| ORD ID | ord-67ad504f42b642f882d4afe7fbafc83d |
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| 出典メモ | uspto-grants-1982_11 |
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