Reaktion #1858318

Reaktionsgleichung

2,6-dimethyl isonicotinic acid

2-amino 2-cyano acetamide

2,6-dimethyl isonicotinyl chloride

→

titled compound

Ausbeute 43.8%

N-(2-amino-1-cyano-2-oxoethyl)-2,6-dimethylisonicotinamide

Ausbeute 43.8%

Lösungsmittel

thionyl chloride

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprepared
2. 2
   Sonstigethionyl chloride was removed in vacuum under nitrogen]
3. 3
   workup.ADDITIONis added at 0° C.
4. 4
   workup.STIRRINGthe reaction mixture is stirred at room temperature for 14 h
5. 5
   Sonstigeafter the completion of the reaction pyridine
6. 6
   Sonstigeis removed under vacuum
7. 7
   Sonstigethe crude product is purified by column chromatography

Vorschrift

2-amino 2-cyano acetamide (1.4 g, 0.01473 mol, 1 eq) in pyridine (15 ml) is stirred for 1 h at room temperature, to this 2,6-dimethyl isonicotinyl chloride (2.5 g, 0.1473 mol, 1 eq) [prepared by stirring a mixture of 2,6-dimethyl isonicotinic acid (2.5 g, 0.0465 mol, 1 eq) in thionyl chloride (15 ml) at 85° C. for 2 hr, thionyl chloride was removed in vacuum under nitrogen] is added at 0° C. and the reaction mixture is stirred at room temperature for 14 h, after the completion of the reaction pyridine is removed under vacuum and the crude product is purified by column chromatography to afford (1.5 g) of the titled compound;

Quelle