2-Amino-6-chloropyridine-3,5-dicarbonitrile → 2-Aminopyridine-3,5-dicarbonitrile

HRID 842705

Reaktionsgleichung

Reaktionsgleichung von HRID 842705
[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

Komponenten

4

Edukt 1

HCID 2959012-Amino-6-chloropyridine-3,5-dicarbonitrile

Produkt 1

HCID 2959122-Aminopyridine-3,5-dicarbonitrile

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

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:

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-a57ce74854b24acfbc7930dae628fd29
Quelldatensatz
uspto-grants-2002_04
Patentnummer
US06376499B1

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