反应详情

To a 5-L round-bottom flask equipped with overhead mechanical stirrer, nitrogen inlet, and thermocouple probe were added 2-acetyl-3-dimethylamino-acrylonitrile (103.65 g, 0.75 mol), anhydrous potassium carbonate (powdered, not granular) (165.85 g, 1.2 mol), and N-[3-(1-methyl-piperidin-4-yl)-propyl]-guanidine (119.02 g, 0.60 mol) in ethanol (2.125 L). The resultant mixture was heated to reflux with stirring and held for 24 h. The resultant mixture was then concentration and the resultant residue partitioned between ethyl acetate (1.5 L) and 1 N NaOH (1.5 L). The layers were separated and the aqueous layer was extracted with additional ethyl acetate (2×1.5 L). The combined organic layers were concentrated to yield the title compound as a solid.

1. customTo a 5-L round-bottom flask equipped with overhead mechanical stirrer, nitrogen inlet
2. temperatureto reflux
3. concentrationconcentration
4. customthe resultant residue partitioned between ethyl acetate (1.5 L) and 1 N NaOH (1.5 L)
5. customThe layers were separated
6. extractionthe aqueous layer was extracted with additional ethyl acetate (2×1.5 L)
7. concentrationThe combined organic layers were concentrated