Hydrochloric Acid → (2,6-Dichloro-5-fluoropyridin-3-yl)methanamine

HRID 40135

Reaktionsgleichung

Reaktionsgleichung von HRID 40135
Cl.[Cl:2][C:3]1[N:10]=[C:9]([Cl:11])[C:8]([F:12])=[CH:7][C:4]=1[C:5]#[N:6]>CO.[Pd]>[Cl:2][C:3]1[C:4]([CH2:5][NH2:6])=[CH:7][C:8]([F:12])=[C:9]([Cl:11])[N:10]=1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 27338492,6-Dichloro-5-fluoro-3-pyridinecarbonitrile

Produkt 1

HCID 55255125(2,6-Dichloro-5-fluoropyridin-3-yl)methanamine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

To a Parr reaction bottle was added Pd—C (10%, 560 mg, 0.52 mmol), followed by 6 M HCl (50 ml) and a solution of 2,6-dichloro-5-fluoronicotinonitrile (Aldrich, 10.0 g, 52.4 mmol) in MeOH (100 ml). The mixture was placed under 50 psi H2 on a shaker type Parr apparatus for 21 h, filtered and concentrated. The crude was dissolved in EtOAc, basified with aqueous NaOH, and the layers were separated. The organic layer was washed with brine, dried over Na2SO4, and concentrated in vacuo to yield the title compound as crude light yellow oil. Used without further purification.

Aufarbeitung

  1. customTo a Parr reaction bottle
  2. filtrationfiltered
  3. concentrationconcentrated
  4. dissolutionThe crude was dissolved in EtOAc
  5. customthe layers were separated
  6. washThe organic layer was washed with brine
  7. dry with materialdried over Na2SO4
  8. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-0f8b145b3d1e4d67813cc531a8167cc1
Quelldatensatz
uspto-grants-2013_09
Patentnummer
US08524917B2

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