HRID1890206

反应详情

EQUATION

反应方程式

HRID 1890206 的结构方程式

PROCEDURE

实验过程

Under an argon atmosphere, 230 g of 1,4-dibromonaphthalene, 121 g of 2-formylphenylboronic acid and 18.5 g of tetraxis(triphenylphosphine)palladium(0) were placed in a flask. 2.4 L of dimethyl ether (DME) and 1.2 L of a 2M aqueous sodium carbonate solution were added to this flask, and the resultant was refluxed with stirring while heating for 8 hours. After cooling to room temperature, an aqueous phase was removed. An organic phase which had been separated was washed with water, and saturated brine, and then dried with magnesium sulfate. After the magnesium sulfate was filtered out, the organic phase was concentrated. The resulting residue was purified by means of silica gel column chromatography, whereby 170 g (yield: 67%) of 1-bromo-4-(2-formylphenyl) naphthalene was obtained.

WORKUP

后处理

  1. temperaturethe resultant was refluxed
  2. temperaturewhile heating for 8 hours
  3. customan aqueous phase was removed
  4. customAn organic phase which had been separated
  5. washwas washed with water, and saturated brine
  6. dry with materialdried with magnesium sulfate
  7. filtrationAfter the magnesium sulfate was filtered out
  8. concentrationthe organic phase was concentrated
  9. customThe resulting residue was purified by means of silica gel column chromatography