反应详情

温度

55 °C

Methyl 6-(3,3-diethoxyprop-1-ynyl)-5-methyl-3-oxo-4-[3-(trifluoromethyl)phenyl]-3,4-dihydropyrazine-2-carboxylate (0.073 g, 0.17 mmol) and 5-hydrazinopyridine-2-carbonitrile trifluoroacetate (0.050 g, 0.20 mmol) in dioxane (3 ml) were placed in a vial. 2M HCl (0.188 ml) was added and the mixture was stirred at 55° C. for 15 min. After cooling, NaHCO3 (0.048 g) was added and the mixture was extracted with DCM and water. The combined organic phases were washed with water, brine, dried (Na2SO4) and evaporated. The residue was dissolved in acetic acid (10 ml) and the vial was sealed. The solution was stirred at 90° C. for 10 h. After evaporation, the residue was purified by preparative HPLC to give 0.023 g (28%) of the title compound.

1. temperatureAfter cooling
2. extractionthe mixture was extracted with DCM and water
3. washThe combined organic phases were washed with water, brine
4. dry with materialdried (Na2SO4)
5. customevaporated
6. dissolutionThe residue was dissolved in acetic acid (10 ml)
7. customthe vial was sealed
8. stirringThe solution was stirred at 90° C. for 10 h
9. customAfter evaporation
10. customthe residue was purified by preparative HPLC