関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Phenylprop-2-enoyl chloride | HCID 66023 | — |
| 反応物 | 2-(2-Aminophenethyl)-1-methylpiperidine | HCID 11085282 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2'-[2-(1-Methyl-2-piperidyl)ethyl]-cinnamanilide | HCID 20981679 | 70% |
反応手順
Cinnamoyl chloride (6.0 g., 0.036 mole) is added to a solution of 2-(o-aminophenethyl)-1-methylpiperidine (7.8 g., 0.036 mole) in 100 ml. of pyridine in one portion with vigorous stirring. Stirring is continued for 3 hours and the pyridine solution is then concentrated in vacuo. The resulting residue is taken up to 150 ml. of water and made basic with 40% sodium hydroxide. The basified solution is extracted with several 200 ml. portions of ether, which are combined, washed with water, dried over magnesium sulfate and the ether solvent evaporated. The residue thus obtained crystallizes and is further purified by crystallizing from isopropyl ether providing 8.7 g. (70% yield) of analytically pure 2'-[2-(1-methyl-2-piperidyl)ethyl]cinnamanilide melting at 101.5°-103.5° C. (corr.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04064254 |
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| 出典データセット | uspto-grants-1977_12 |
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| ORD ID | ord-d3e79ec021ae40d7a9dc9a5ae9aca0a5 |
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| 出典メモ | uspto-grants-1977_12 |
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