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 4-Chloro-7-isopropyl-7H-imidazo[4,5-c]pyridazine (Preparation 6, 50 mg, 0.254 mmoles) and 2′-fluoro-5′-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)biphenyl-4-sulfonamide (Preparation 2, 131 mg, 0.254 mmoles) in dioxane (2.5 mL) was added Na2CO3 (80 mg, 0.759 mmol) pre dissolved in water (0.5 mL) and [1,1-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (7.3 mg, 0.009 mmol). The reaction was degassed with nitrogen and heated under microwave irradiation at 90° C. for 15 minutes. After cooling, ethyl acetate and Na2SO4 were added and the mixture decanted and washed with ethyl acetate. Purification by silica gel column chromatography eluting with DCM: MeOH 1:0 to 9:1 yielded the title product in 50% yield, 57 mg.
WORKUP
后处理
- customThe reaction was degassed with nitrogen
- temperatureAfter cooling
- additionethyl acetate and Na2SO4 were added
- customthe mixture decanted
- washwashed with ethyl acetate
- customPurification by silica gel column chromatography
- washeluting with DCM: MeOH 1:0 to 9:1