関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 反応物 | Ethyl nipecotate | HCID 98969 | — |
| 反応物 | 4-(Carboxymethyloxy)-4'-cyano-biphenyl | HCID 43243100 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Cyano-4'-[[(3-ethoxycarbonylpiperidino)carbonyl]methyloxy]biphenyl | HCID 53802755 | — |
反応手順
5.35 g of carbonyldiimidazole are added to a solution of 7.6 g of 4-(carboxymethyloxy)-4'-cyano-biphenyl (prepared from 4-cyano-4'-hydroxy-biphenyl and tert.butyl bromoacetate according to Example 13, but with potassium tert.butoxide as base, and subsequent ester cleaving with trifluoroacetic acid) in 30 ml of tetrahydrofuran and the resulting mixture is stirred for 0.5 hours at ambient temperature. 5.1 ml of ethyl piperidine-3-carboxylate are added and the mixture is stirred for 22 hours at ambient temperature. The tetrahydrofuran is evaporated off, the residue is taken up in ethyl acetate and washed successively with saturated sodium bicarbonate solution, 0.1N hydrochloric acid and water. After evaporation of the organic phase the residue remains as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05922763 |
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| 出典データセット | uspto-grants-1999_07 |
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| ORD ID | ord-08e265ac59d04f618b42a0a0df0376a1 |
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| 出典メモ | uspto-grants-1999_07 |
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