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1-Methylpiperazine → 5-((4-Methylpiperazine-1-yl)methyl)furan-2-carboxaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 反応物 | 5-(Bromomethyl)-2-furaldehyde | HCID 11970491 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 5-((4-Methylpiperazine-1-yl)methyl)furan-2-carboxaldehyde | HCID 86671381 | 55% |
反応手順
To a solution of 0.20 g (1.1 mmol) of 5-(bromomethyl)furan-2-carboxaldehyde in anhydrous dioxane (10 ml) are added 261 μL (0.24 g, 2.3 mmol) of 1-methylpiperazine. The mixture is stirred at room temperature for 30 min. The precipitate formed is filtered and rinsed with dioxane. The filtrate is concentrated, dissolved in dichloromethane, and washed in water. The organic phase is dried over magnesium sulfate, filtered, and concentrated. The residue obtained is purified by chromatography on silica (eluent: 7N NH4OH in MeOH/CH2Cl2, 5:95) to yield 0.12 g (55%) of 5-((4-methylpiperazine-1-yl)methyl)furan-2-carboxaldehyde in the form of an orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08889711B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-c4556eb69876429c80231218238a6038 |
| 出典メモ | uspto-grants-2014_11 |