化工社化工社 化学情報印刷レポート · 研究参考用
p-Fluoronitrobenzene → 1-(4-Nitrophenyl)piperidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Fluoronitrobenzene | HCID 9590 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Piperidone hydrochloride | HCID 3084851 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 生成物 | 1-(4-Nitrophenyl)piperidin-4-one | HCID 3842562 | 37% |
反応手順
Piperidin-4-one hydrochloride was added to a methanolic solution of sodium methoxide (prepared from anhydrous methanol (50 mL) and sodium metal (0.85 g, 37 mmol)) and heated at reflux for 2 h then concentrated to dryness in vacuo. The residue was dissolved in acetonitrile (100 mL), then potassium carbonate (10.22 g, 74 mmol) and 1-fluoro-4-nitro-benzene (3.92 mL, 37 mmol) were added and the mixture was heated at reflux overnight. The solvent was evaporated in vacuo, the residue being washed with water then 50% diethyl ether/petroleum ether and dried in vacuo to afford 1-(4-nitro-phenyl)-piperidin-4-one (3.01 g, 37%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524705B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-49e8b3dab6e44043b8dc93c7ea9a469e |
| 出典メモ | uspto-grants-2013_09 |