反应详情

2-Chlorobenzaldehyde (0.3 g, 2.12 mmole), N-(pyrid-2-yl)-3-aminocrotonamide (0.38 g, 2.12 mmole) (obtained from N-(pyrid-2-yl)-3-oxobutanamide by reaction with ethanolic ammonia at room temperature for 16 hours) and ethyl 4-[2-(3-methyl-5-phenyl-4H-1,2,4-triazol-4-yl)ethoxy]-3-oxobutanoate (0.7 g, 2.12 mmole) were dissolved in absolute ethanol (25 ml) and the mixture heated under reflux for 5 hours. The solution was cooled and concentrated to dryness under reduced pressure. The residue was chromatographed on silica, eluting with ethyl acetate containing 15% ethanol. Appropriate fractions were combined, concentrated under vacuum and the residue triturated with ethyl acetate to yield the title product as a white amorphous solid (0.23 g, 20%), m.p. 167°-169° C. Found: C,64.92; H,5.61; N,13.39. C33H33ClN6O4 requires C,64.65; H,5.43; N,13.71%.

1. temperaturethe mixture heated
2. temperatureunder reflux for 5 hours
3. temperatureThe solution was cooled
4. concentrationconcentrated to dryness under reduced pressure
5. customThe residue was chromatographed on silica
6. washeluting with ethyl acetate containing 15% ethanol
7. concentrationconcentrated under vacuum
8. customthe residue triturated with ethyl acetate