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Piperazine → 1-(3-Methyl-2-pyridinyl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | 2-Bromo-3-methylpyridine | HCID 220832 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 1-(3-Methyl-2-pyridinyl)piperazine | HCID 2760057 | — |
反応手順
To a slurry of 2-bromo-3-methylpyridine (3.30 mL, 29.6 mmol) in n-butanol was added piperazine (25.0 g, 290 mmol) and the reaction heated to reflux for 3 days. The mixture was cooled and the solvent removed under reduced pressure. The residue was partitioned between water and ethyl acetate. The organic phase was dried (sodium sulfate) and concentrated. The residue was purified by flash column chromatography on silica gel (elution with 15% methanol:dichloromethane) to provide the title compound as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07528134B2 |
| 出典データセット | uspto-grants-2009_05 |
| ORD ID | ord-574248bc234740a2bbf0875f2d8c86bc |
| 出典メモ | uspto-grants-2009_05 |