反应详情

温度

150 °C

6-Bromo-5-(2,4-difluorophenoxy)-1-isobutyl-1H-indazole (31.2 g, 82 mmol) and Cu(I)CN (13.9 g, 156 mmol) were dissolved in DMA and degassed with nitrogen under vacuum. The reaction mixture was heated to 150° C. for 16 hours. The mixture was then cooled to room temperature and diluted with ethyl acetate before washing twice with 7M NH4OH. The organic layer was washed with brine and degassed with nitrogen before being dried over MgSO4 and concentrated under reduced pressure. The crude product was chromatographed eluting with 10% ethyl acetate in hexanes to afford 25.1 g of the desired product (95% yield).

1. customdegassed with nitrogen under vacuum
2. temperatureThe mixture was then cooled to room temperature
3. additiondiluted with ethyl acetate
4. washbefore washing twice with 7M NH4OH
5. washThe organic layer was washed with brine
6. customdegassed with nitrogen
7. dry with materialbefore being dried over MgSO4
8. concentrationconcentrated under reduced pressure
9. customThe crude product was chromatographed
10. washeluting with 10% ethyl acetate in hexanes