化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → (E)-1-[4-(3-Methoxy-2-methyl-4-pyridyl)piperazin-1-yl]-4-methyl-pent-2-en-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (E)-4-methylpent-2-enoyl Chloride | HCID 10986269 | — |
| 反応物 | 1-(3-Methoxy-2-methyl-4-pyridyl)piperazine | HCID 66835613 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (E)-1-[4-(3-Methoxy-2-methyl-4-pyridyl)piperazin-1-yl]-4-methyl-pent-2-en-1-one | HCID 56949086 | 7% |
反応手順
1-(3-Methoxy-2-methyl-4-pyridyl)piperazine (20.7 mg, 0.1 mmol) was dissolved in dichloromethane (1 ml), triethylamine was added (1 ml of a 0.12 M solution in dichloromethane) followed by a solution of (E)-4-methylpent-2-enoyl chloride (1 ml, 0.12 M in dichloromethane). The mixture was shaken briefly, washed with 5% sodium bicarbonate solution (2×), water and evaporated to dryness. The raw product was purified by preparative HPLC (gradient of water containing 0.1% ammonia and acetonitrile) to yield 2.2 mg of a solid (0.007 mmol, 7%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08883791B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-ca634ec73b514dff8534f717029a5b91 |
| 出典メモ | uspto-grants-2014_11 |