関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | (3-Bromopropyl)benzene | HCID 12503 | — |
| 反応物 | 3-(R,S)-(1-cyano-1,1-diphenylmethyl)piperidine | HCID 13633746 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(R,S)-(1-cyano-1,1-diphenylmethyl)-1-(3-phenylpropyl)piperidine | HCID 21224086 | — |
反応手順
A mixture containing 3-(R,S)-(1-cyano-1,1-diphenylmethyl)piperidine (0.3 g--see EP-A-0178947), 1-bromo-3-phenylpropane (0.238 g), anhydrous potassium carbonate (0.4 g) and acetonitrile (10 ml) was heated under reflux for 5 hours. The mixture was partitioned between dichloromethane (30 ml) and 10% aqueous potassium carbonate (30 ml), the layers separated, and the aqueous layer extracted with dichloromethane (2×20 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated vacuo to give a gum which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 2%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a gum, yield 0.4g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05422358 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-d567ec4934e94bc8972791d5770869a0 |
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| 出典メモ | uspto-grants-1995_06 |
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