HRID1845988

反应详情

EQUATION

反应方程式

HRID 1845988 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. customThe reaction was degassed with nitrogen
  2. temperatureAfter cooling
  3. additionethyl acetate and Na2SO4 were added
  4. customthe mixture decanted
  5. washwashed with ethyl acetate
  6. customPurification by silica gel column chromatography
  7. washeluting with DCM: MeOH 1:0 to 9:1