2-Pyrazinecarbonitrile, 3-azido-6-fluoro- → HCID 22662784, Verbindung

HRID 392347

Reaktionsgleichung

Reaktionsgleichung von HRID 392347
[N:1]([C:4]1[C:5]([C:11]#[N:12])=[N:6][C:7]([F:10])=[CH:8][N:9]=1)=[N+]=[N-].[H][H]>CO.C(=O)([O-])[O-].[Ca+2].[Pd+2].C(=O)([O-])[O-]>[NH2:1][C:4]1[C:5]([C:11]#[N:12])=[N:6][C:7]([F:10])=[CH:8][N:9]=1

Komponenten

5

Edukt 2

HCID 226627892-Pyrazinecarbonitrile, 3-azido-6-fluoro-HCID 178418361HCID 178418361, Verbindung2×

Produkt 1

HCID 22662784HCID 22662784, VerbindungAusbeute 38,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 17803853Palladium on calcium carbonateKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

In 5.0 mL of methanol was dissolved 0.24 g of 3-azido-6-fluoro-2-pyrazinecarbonitrile. After adding 0.075 g of lead-poisoned palladium-calcium carbonate at room temperature, hydrogen gas was introduced into the mixture at room temperature under a pressure of 1 atmosphere until the mixture became showing no further adsorption of hydrogen. After filtering off the insoluble matter from the reaction mixture, the filtrate was concentrated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent: chloroform] to obtain 0.078 g of 3-amino-6-fluoro-2-pyrazinecarbonitrile as a yellow-colored solid product.

Aufarbeitung

  1. filtrationAfter filtering off the insoluble matter from the reaction mixture
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue thus obtained
  4. customwas purified by silica gel column chromatography [eluent: chloroform]

Quellen und Nachweise

ORD-Eintrag
ord-4480d28c37a24f63a3f2cd8e179bbf7d
Quelldatensatz
uspto-grants-2004_10
Patentnummer
US06800629B2

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