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2-氨基-6-氯-3,5-二氰基吡啶 → 3,5-二氰基-3-氨基吡啶
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 2-氨基-6-氯-3,5-二氰基吡啶 | HCID 295901 | — |
| 催化剂 | 钯 | HCID 23938 | — |
| 溶剂 | 1,4-二氧六环 | HCID 31275 | — |
| 产物 | 3,5-二氰基-3-氨基吡啶 | HCID 295912 | — |
反应步骤
A mixture of 2-amino-6-chloro-3,5-dicyanopyridine (Synth. Comm. 1993, 2605, 15.0 g, 84 mmol) and 10% palladium on carbon (10.0 g) in dioxane (150 mL) was shaken on a Parr apparatus under hydrogen (55 psi) for 16 h. More catalyst (7.5 g) was added and after a further 4 h the reaction mixture was filtered through celite washing through with ethanol and evaporated in vacuo. The residue was partitioned between methylene chloride and 1 M HCl. The insoluble material was collected by filtration and dried to give the title compound. The methylene chloride layer was washed with brine, dried (Na2SO4) and evaporated in vacuo to give additional product:
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US06376499B1 |
| 来源数据集 | uspto-grants-2002_04 |
| ORD ID | ord-a57ce74854b24acfbc7930dae628fd29 |
| 来源说明 | uspto-grants-2002_04 |