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N,N-dimethyl-6-nitropyridin-3-amine → N5,N5-Dimethylpyridine-2,5-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N-dimethyl-6-nitropyridin-3-amine | HCID 21897368 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N5,N5-Dimethylpyridine-2,5-diamine | HCID 5743468 | — |
反応手順
The N,N-dimethyl-6-nitropyridine-3-amine obtained above is taken up in 25 ml of ethanol. After addition of 4.8 g of stannous chloride, the reaction mixture is heated at reflux for 30 minutes and then concentrated to dryness. The residue is chromatographed on a column of silica (40-63 μm), elution being carried out with a mixture of dichloromethane and ammoniacal methanol (90/10). The fractions comprising the expected product are combined and concentrated to give 750 mg of 5-dimethylaminopyridine-2-amine in the form of a pasty yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07704989B2 |
| 出典データセット | uspto-grants-2010_04 |
| ORD ID | ord-0d3391d71d19420b8014b85f19f742cb |
| 出典メモ | uspto-grants-2010_04 |