反应详情

温度

40 °C

1-Methyl-2-pyrrolecarboxylic acid (1.49 g, 11.9 mmol) was dissolved in methylene chloride (12 mL) and the solution was added with thionyl chloride (1.3 mL, 17.85 mmol) and DMF (276 μL, 3.57 mmol) at 0° C., stirred at 40° C. for 2 hours and then the mixture was concentrated. The mixture was dissolved in THF, added with a solution of (E)-2-[2-(1H-indazol-3-yl)vinyl]phenylamine (700 mg, 2.98 mmol) and triethylamine (1.25 mL, 8.93 mmol) in THF (10 mL) at room temperature, stirred at 60° C. for 4 hours. Further, potassium carbonate and methanol (10 mL) were added to the mixture and stirred for a while and then added with water. The precipitated solid was collected by filtration and reslurried with ethanol to obtain Compound 29 (703 mg, 69%).

1. concentrationthe mixture was concentrated
2. dissolutionThe mixture was dissolved in THF
3. stirringstirred at 60° C. for 4 hours
4. stirringstirred for a while
5. filtrationThe precipitated solid was collected by filtration