Reaktion #1963938

Reaktionsgleichung

3-Oxo-butyronitrile

DMF-DMA

→

title compound

(E)-2-[(dimethylamino)-methylene]-3-oxobutanenitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvents were then removed under vacuum
2. 2
   Sonstigeto yield a solid
3. 3
   SonstigeThe solid was partitioned between ethyl acetate (1.5 L) and saturated sodium bicarbonate solution (1 L)
4. 4
   SonstigeThe layers were separated
5. 5
   Extraktionthe aqueous layer was extracted with ethyl acetate (1.5 L)
6. 6
   Sonstigethe solvent removed under vacuum

Vorschrift

3-Oxo-butyronitrile (113 g, 1.36 mol) and DMF-DMA (215 g, 1.81 mol) were heated to 80° C. for two hours. The solvents were then removed under vacuum to yield a solid. The solid was partitioned between ethyl acetate (1.5 L) and saturated sodium bicarbonate solution (1 L). The layers were separated and the aqueous layer was extracted with ethyl acetate (1.5 L). The organic layers were combined and the solvent removed under vacuum to yield the title compound as a solid.

Quelle