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Water → 1-(4-Benzoylphenyl)-4-(4-pyridyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Fluorobenzophenone | HCID 67663 | — |
| 反応物 | 1-(4-Pyridyl)piperazine | HCID 70517 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-(4-Benzoylphenyl)-4-(4-pyridyl)piperazine | HCID 18357129 | 26.2% |
反応手順
A solution of N-(4-pyridyl)piperazine (815 mg), 4-fluorobenzophenone (1.2 g) and powdered potassium carbonate (912 mg) was stirred at 95° C. in DMSO (10 ml) overnight. The solution was poured into water (150 ml) and extracted with dichloromethane (3×50 ml). The dichloromethane extracts were combined, washed with water, dried (Na2SO4) and evaporated. The residue was purified by chromatography on alumina (ICN Alumina N 32-63) using 1% methanol in dichloromethane as eluant to give a solid. The solid was recrystallised from a mixture of ethyl acetate/isohexane to give 1-(4-benzoylphenyl)-4-(4-pyridyl)piperazine (450 mg) as a solid. m.p.136-137° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06313127B1 |
| 出典データセット | uspto-grants-2001_11 |
| ORD ID | ord-f727f45183664540b591d773fc72606e |
| 出典メモ | uspto-grants-2001_11 |