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Triethylamine → 3-[4-(4-Hydroxy-phenyl)-piperazin-1-yl]-butyric acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Butanoic acid, 3-bromo-, methyl ester | HCID 89470 | — |
| 反応物 | p-(1-Piperazinyl)phenol | HCID 92467 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-[4-(4-Hydroxy-phenyl)-piperazin-1-yl]-butyric acid methyl ester | HCID 68432675 | 59.3% |
反応手順
To a mixture of 4-piperazin-1-yl-phenol (2 g, 11.2 mmol) and methyl 3-bromo-butyrate (2.03 g, 11.2 mmol) in DMF (5 mL) was added triethylamine (4.5 mL, 11.53 mmol) dropwise and the reaction mixture was stirred at ambient temperature overnight. The mixture was poured onto water and extracted with ethyl acetate (50 ml×3). The combined organic layers were washed with brine, dried over anhydrous Na2SO4 and evaporated under vacuum to dryness. The residue was purified by silica gel flash chromatography (1% methanol in CH2Cl2) to furnish the title compound (1.85 g, 59.3%); MS; m/z 279 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728032B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-8b0039b8c75446b48104676c801868df |
| 出典メモ | uspto-grants-2010_06 |