反应详情

To a solution of 5-(benzyloxy)-6-bromo-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole (4 g, 10.3 mmol) in 1,4-dioxane (25 mL) is added bis(pinacolato)diboron (3 g, 11.8 mmol), dppf (0.3 g, 541 μmol), PdCl2(dppf) (0.42 g, 514 μmol) and KOAc (2 g, 20.4 mmol) under N2. After the reaction mixture is stirred at reflux for 5 hours, 5-bromo-2-methylpyridine (2.1 g, 12.2 mmol), tetrakis(triphenylphosphine)palladium (Pd(PPh3)4) (0.6 g, 519 μmol) and Cs2CO3 (4 g, 12.3 mmol) are added and the mixture is stirred at reflux overnight. The reaction mixture is cooled and filtered, the filtrate is concentrated. The residue is purified by silica gel column chromatography eluting with PE:EtOAc (2:1) to give the product (1.9 g, 46.0% yield). MS (m/z): 400.1 (M+H).

1. temperatureat reflux for 5 hours
2. stirringthe mixture is stirred
3. temperatureat reflux overnight
4. temperatureThe reaction mixture is cooled
5. filtrationfiltered
6. concentrationthe filtrate is concentrated
7. customThe residue is purified by silica gel column chromatography
8. washeluting with PE