2-氨基-6-氯-3,5-二氰基吡啶 → 3,5-二氰基-3-氨基吡啶

HRID 842705

反应方程式

HRID 842705 反应方程式
[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]#[N:11])=[C:4](Cl)[N:3]=1>[Pd].O1CCOCC1>[NH2:1][C:2]1[C:7]([C:8]#[N:9])=[CH:6][C:5]([C:10]#[N:11])=[CH:4][N:3]=1

参与物

4

反应物 1

HCID 2959012-氨基-6-氯-3,5-二氰基吡啶

产物 1

HCID 2959123,5-二氰基-3-氨基吡啶

试剂、催化剂与溶剂 2

HCID 23938钯催化剂HCID 312751,4-二氧六环溶剂

实验过程

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:

后处理

  1. filtrationwas filtered through celite
  2. washwashing through with ethanol
  3. customevaporated in vacuo
  4. customThe residue was partitioned between methylene chloride and 1 M HCl
  5. filtrationThe insoluble material was collected by filtration
  6. customdried

来源与证据

ORD记录
ord-a57ce74854b24acfbc7930dae628fd29
来源数据集
uspto-grants-2002_04
专利号
US06376499B1

关联笔记

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