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Potassium Carbonate → Methyl 4-(4-methylpiperazin-1-yl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 反応物 | Methyl 4-fluorobenzoate | HCID 67878 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Methyl 4-(4-methylpiperazin-1-yl)benzoate | HCID 1472668 | — |
反応手順
4-Fluorobenzoic acid methyl ester (34 mmol), 1-methyl-piperazine (75 mmol) and potassium carbonate (34 mmol) are suspended in acetonitrile (30 ml) and stirred under reflux for three days. After evaporation of the solvent, the residue is dissolved in water and extracted three times with ethyl acetate. The extract is dried over sodium sulfate and evaporated. The residue is purified by flash chromatography on silica gel with (CH2Cl2/MeOH=95:5) as mobile phase. The product containing fractions are combined and evaporated. The residue is suspended in diethylether/pentane and the solid filtered of and dried (vacuum). A pale yellow powder with mp. 117-119° C., Rf=0.20 (CH2Cl2/MeOH=95:5) is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06642239B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-f8e68535ffe6496eb0ba31d65120bc69 |
| 出典メモ | uspto-grants-2003_11 |