関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl ethylmalonate | HCID 8610 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-(Bromomethyl)-2-phenylbenzene | HCID 263365 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(2-Biphenylyl)-2-ethylpropionic acid | HCID 21571983 | 93% |
反応手順
188 g (1 mol) of diethyl ethylmalonate dissolved in 100 cm3 of H2O-free EtOH are added dropwise at room temperature to 23 g (1 mol) of sodium in 400 cm3 of H2O-free EtOH. 247 g (1 mol) of 2-phenylbenzyl bromide in 300 cm3 of H2O-free EtOH were subsequently added dropwise, and the mixture was refluxed for 3 hours. 170 g (3 mol) of KOH dissolved in 300 cm3 of H2O were added at room temperature, and the mixture was refluxed for a further 4 hours. The solvent was removed in vacuo, H2O was added to the residue until the latter had dissolved completely, and the mixture was subsequently acidified to pH 1 by means of concentrated aqueous HCl. The precipitate which formed was filtered off with suction, dried and heated at 130° C. for 1 hour, giving 236 g (93%) of 13 as a viscous oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06051727 |
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| 出典データセット | uspto-grants-2000_04 |
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| ORD ID | ord-524b6156d7d0407088a9f76a0254d3e6 |
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| 出典メモ | uspto-grants-2000_04 |
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