関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 2-Methylpentanedinitrile | HCID 20686 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 生成物 | 3-Methylpyridine-2,6-diamine | HCID 103907 | — |
反応手順
2-Methylglutaronitrile was combined with Pd.C (5 mol % of 10 wt % Pd on carbon) in a 10 mL Hastelloy shaker autoclave to which liquid NH3 was added. The mixture was heated at 200° C. for 45 h. The mixture was cooled to ambient temperature and the excess NH3 removed by N2 purge. The crude mixture was suspended in 10 mL anhydrous methanol, the catalyst was removed by syringe filtration, and the crude reaction mixture was concentrated in vacuo. 2-Methylglutaronitrile conversion was 100% to give 0.02 mmol of 3-methylpyridine-2,6-diamine in 2.3% net yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08022167B2 |
|---|
| 出典データセット | uspto-grants-2011_09 |
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| ORD ID | ord-7111e65421014e1b85ed2eaa4bf285da |
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| 出典メモ | uspto-grants-2011_09 |
|---|