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Ammonia → Bis(2-pyridyl)methylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Di-2-pyridinylmethanone oxime | HCID 73805 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Bis(2-pyridyl)methylamine | HCID 11106041 | 86% |
反応手順
To pyridyl ketone oxim (3 g, 15.1 mmol) was added ethanol (15 ml), concentrated ammonia solution (15 mL) and NH4OAc (1.21 g, 15.8 mmol). The solution was warmed until reflux. To this solution was added 4.64 g Zn in small portions. After the addition of all Zn, the mixture was refluxed for 1 hour and allowed to cool to ambient temperature. The solution was filtered and water (15 ml) was added. Solid NaOH was added until pH>>10 and the solution was extracted with CH2Cl2 (3×20 ml). The organic layers were dried over Na2SO4 and evaporated until dryness. Bis(pyridin-2-yl)methylamine (2.39 g, 12.9 mmol) was obtained as a colourless oil in 86% yield, showing the following analytical characteristics:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06242409B1 |
| 出典データセット | uspto-grants-2001_06 |
| ORD ID | ord-cd8d159658c44b6aaaee908c220b336a |
| 出典メモ | uspto-grants-2001_06 |