反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
To a mixture of 1-(trans-4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-5-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (202.16 mg, 0.48079 mmol), Potassium fluoride (76.18 mg, 1.311 mmol) and 3-[2,2-Bis-benzenesulfonyl-1-(2,6-dichloro-3-fluoro-phenyl)-2-fluoroethyl]-5-bromo-1H-pyrrolo[2,3-b]pyridine (300.00 mg, 0.43708 mmol) in 1,4-Dioxane (10.00 mL, 128.1 mmol) and H2O (2.500 mL, 138.8 mmol) was added (1,1′-bis-(diphenylphosphino)-ferrocene) palladium dichloride (15.99 mg, 0.02185 mmol) under Nitrogen atmosphere, the resulting mixture was then stirred at 90° C. for 90 min. Then the solvent was removed under reduced pressure to give a residue, which was purified by silica gel chromatography (eluent: 20-30% AcOEt in DCM) to give the title compound. MS (ES+): m/z 899.20, 901.21 [MH+]. HPLC: tR=1.98 min (polar—3 min, TOF).
WORKUP
后处理
- customThen the solvent was removed under reduced pressure
- customto give a residue, which
- customwas purified by silica gel chromatography (eluent: 20-30% AcOEt in DCM)