関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Chloromethyl-2-(3,4,5-trimethoxyphenyl) pyridine | HCID 12019237 | — |
| 反応物 | 2-Oxo-1-[[2-(3,4,5-trimethoxyphenyl)pyridin-4-yl]methyl]piperazine | HCID 12019238 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 2-oxo-N,N'-bis[[2-(3,4,5-trimethoxyphenyl)-pyridin-4-yl]methyl]piperazine | HCID 10282496 | — |
反応手順
2-Oxo-1-[[2-(3,4,5-trimethoxyphenyl)pyridin-4-yl]methyl]piperazine (62 mg) was dissolved in acetonitrile (5 mL), and to the solution potassium carbonate (24 mg), potassium iodide (29 mg) and 4-chloromethyl-2-(3,4,5-trimethoxyphenyl)pyridine (51 mg) were added, and the mixture was stirred at 80° C. for 1 hour. The reaction mixture was concentrated under reduced pressure, ethyl acetate was added to the residue, and the resultant mixture was washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resultant oil was purified by preparative TLC on silica gel (chloroform:methanol=25:1) to obtain the title compound as a hydrochloride.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06432957B1 |
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| 出典データセット | uspto-grants-2002_08 |
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| ORD ID | ord-4d375eaacbbf42328d35fa5d9a4f573d |
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| 出典メモ | uspto-grants-2002_08 |
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