反应详情

温度

90 °C

To a solution of 5-(2,6-difluorophenyl)-3-iodo-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole 14 (0.2 g, 0.45 mmol) and 2-Chloro-4-tributylstannanyl-pyrimidine 20a (0.27 g, 0.68 mmol) in DMF was bubbled N2 for 15 min and added CuI (0.052 g, 0.54 mmol) and Pd(PPh3)4 (0.1 g, 0.025 mmol). The reaction mixture was heated at 90° C. for 2 h and cooled to RT. The reaction mixture was quenched with water and precipitate was formed. The resulting precipitate was collected by filtration, washed with water, and dried to yield crude product. Purification by silica gel column chromatography, eluting with 5-10% EtOAc and hexanes to obtain the title compound (0.1 g, 38%). MS (ESI, pos. ion) m/z: 427.0 (M+1).

1. temperaturecooled to RT
2. customThe reaction mixture was quenched with water
3. customprecipitate was formed
4. filtrationThe resulting precipitate was collected by filtration
5. washwashed with water
6. customdried
7. customto yield crude product
8. customPurification by silica gel column chromatography
9. washeluting with 5-10% EtOAc and hexanes