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Allyl bromide → Ethyl trans-4-allyl-2,5-dimethyl-1-piperazinecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Allyl bromide | HCID 7841 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Ethyl trans-2,5-dimethyl-1-piperazinecarboxylate | HCID 10607598 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Ethyl trans-4-allyl-2,5-dimethyl-1-piperazinecarboxylate | HCID 10823138 | 81% |
反応手順
A mixture of ethyl trans-2,5-dimethyl-1-piperazinecarboxylate (643 g, 3.45 mol), allyl bromide (328 mL, 3.80 mol), and sodium carbonate (440 g, 4.15 mol) in 2500 mL of acetonitrile was heated at reflux for 1.5 hours. The reaction was cooled to room temperature, filtered, and the solvent removed under vacuum. The residue was dissolved in 4000 mL of dichloromethane and washed with two 500 mL portions of 1 M sodium hydroxide. The dichloromethane solution was dried over magnesium sulfate and the solvent was removed to give 630 g (81%) of ethyl trans-4-allyl-2,5-dimethyl-1-piperazinecarboxylate as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08865721B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-b43049bded6b4709bf76bcaf281c51f6 |
| 出典メモ | uspto-grants-2014_10 |