HRID571057

反应详情

EQUATION

反应方程式

HRID 571057 的结构方程式

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

To a 20 mL microwave vial (Biotage) was added {3-[(4-methoxybenzyl)oxy]-4-oxo-4H-1,2′-bipyridin-4′-yl}boronic acid (300 mg, 0.85 mmol), iodobenzene (348 mg, 1.70 mmol), cesium carbonate (6 mL of a 1.0 M aq solution, 6.0 mmol), and 69.6 mg (0.085 mmol) 1,1′-bis(diphenylphosphino)ferrocene-palladium(II)dichloride dichloromethane complex. The vial was sealed and the reaction mixture was heated at 135° C. under microwave irradiation for 15 minutes, then cooled. The organic layer was separated, washed with 5 mL water, dried over Na2SO4, filtered, and concentrated in vacuo. Purification by flash chromatography (silica gel, 0-10% MeOH in EtOAc gradient) afforded 3-[(4-methoxybenzyl)oxy]-4′-phenyl-4H-1,2′-bipyridin-4-one. LCMS (M+H)+=385.4.

WORKUP

后处理

  1. customThe vial was sealed
  2. temperaturecooled
  3. customThe organic layer was separated
  4. washwashed with 5 mL water
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customPurification by flash chromatography (silica gel, 0-10% MeOH in EtOAc gradient)