反应详情

91 mg (0.936 mmol) cyclopentane-1,3-dione, 150 mg (0.936 mmol) 3-methyl-1H-indazole-5-carbaldehyde (Example 1A) and piperidine (0.1 ml) in ethanol (8 ml) were heated to reflux for 1.5 h and then left standing without stirring at room temperature overnight. The mixture was then evaporated to dryness, the remaining solid was dissolved in acetic acid (8 ml), and 77 mg (0.936 mmol) 3-aminobut-2-enenitrile were added. The solution was heated to reflux for 2 h. After cooling, the mixture was evaporated to dryness again, and the remaining solid was purified by preparative RP-HPLC (acetonitrile/water gradient) to yield 34 mg (12% of th.) of the title compound.

1. temperatureto reflux for 1.5 h
2. waitleft standing
3. customThe mixture was then evaporated to dryness
4. dissolutionthe remaining solid was dissolved in acetic acid (8 ml)
5. temperatureThe solution was heated
6. temperatureto reflux for 2 h
7. temperatureAfter cooling
8. customthe mixture was evaporated to dryness again
9. customthe remaining solid was purified by preparative RP-HPLC (acetonitrile/water gradient)