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p-Fluoronitrobenzene → 1-Benzyl-4-(4-nitrophenyl)piperazine
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 | 1-Benzylpiperazine | HCID 75994 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Benzyl-4-(4-nitrophenyl)piperazine | HCID 2747427 | 57% |
反応手順
A stirred solution of 1-benzylpiperazine (8.81 g, 50.0 mmol), 4-fluoronitrobenzene (5.31 mL, 50.0 mmol), and K2CO3 (6.90 g, 50.0 mmol) in ethanol is heated at reflux temperature under nitrogen for 18 h, cooled, diluted with water, and extracted with CH2Cl2. The combined extracts are dried over MgSO4 and concentrated in vacuo to give a solid residue. The solid is triturated with 20:80 ethyl acetate:hexanes and filtered. The filtercake is air-dried to afford the title compound as orange crystals, 8.45 g (57% yield), mp 218-219° C., characterized by NMR and mass spectral analyses.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560470B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-72b38b2b4147411cabcc88502678d0b8 |
| 出典メモ | uspto-grants-2009_07 |