反应详情

温度

100 °C

To a solution of 3,5-dibromo-2-methylpyridine (320 mg, 1.28 mmol) in dioxane (10 mL), was added 1-methyl-5-(tributylstannyl)-1H-pyrazolo[4,3-b]pyridine (540 mg, 1.28 mmol), CuI (73 mg, 0.38 mmol), LiCl (271 mg, 6.4 mmol) and Pd(PPh3)4 (147 mg, 0.12 mmol). The reaction mixture was heated at 100° C. for 2 h. The reaction was cooled down, washed by sat. NaHCO3, extracted by EtOAc, dried over MgSO4, filtered, concentrated down and purified by silica gel column, eluting by 0-100% EtOAc in hexanes give the product. LCMS-ESI+: calc'd for C13H11BrN4: 303.0 (M+H+); Found: 303.2 (M+H+).

1. temperatureThe reaction was cooled down
2. washwashed by sat. NaHCO3
3. extractionextracted by EtOAc
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated down
7. custompurified by silica gel column
8. washeluting by 0-100% EtOAc in hexanes
9. customgive the product