HRID1661893

反应详情

EQUATION

反应方程式

HRID 1661893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 100 mg (0.25 mmol) 4-bromo-2-(4-isopropyl-phenyl)-7-methoxy-1-(2-methoxy-ethyl)-1H-benzoimidazole, 45 mg (0.424 mmol) sodium carbonate, 34 mg (0.275 mmol) phenyl-boronic acid and 10 mg tetrakis(triphenylphosphine) palladium in 10 ml toluene/water (3:1) is stirred at 100° C. for 9 hours. Then the reaction mixture is cooled to room temperature and poured on water and extracted (3×) with ethyl acetate. The combined organic layers are washed with water (2×) and brine, dried over MgSO4, filtered and concentrated in vacuo. The residue is purified by flash-chromatography on silica gel (hexane:EtOAc=4:1) to afford 53 mg of the title compound as a white crystalline solid.

WORKUP

后处理

  1. temperatureThen the reaction mixture is cooled to room temperature
  2. additionpoured on water
  3. extractionextracted (3×) with ethyl acetate
  4. washThe combined organic layers are washed with water (2×) and brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue is purified by flash-chromatography on silica gel (hexane:EtOAc=4:1)