HRID1096987

反应详情

EQUATION

反应方程式

HRID 1096987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Methyl 3,5-dimethoxy-4-bromobenzoate (500 mg) was dissolved in toluene in a nitrogen atmosphere, and 1-ethoxyvinyltributyltin (742 μL) and tetrakis(triphenylphosphine)palladium (211 mg) were added to it, and stirred overnight at 110° C. The reaction liquid was cooled to room temperature, then aqueous potassium fluoride solution was added to it, and stirred at room temperature. The reaction liquid was filtered through Celite, the Celite was washed with ethyl acetate, and the filtrate was washed with saturated saline water. The organic layer was dried with sodium sulfate, the sodium sulfate was removed through filtration, the filtrate was concentrated under reduced pressure, and the residue was purified through silica gel column chromatography (hexane/ethyl acetate=100/0 to 85/15) to obtain the title compound.

WORKUP

后处理

  1. additionwere added to it
  2. customThe reaction liquid
  3. temperaturewas cooled to room temperature
  4. stirringstirred at room temperature
  5. customThe reaction liquid
  6. filtrationwas filtered through Celite
  7. washthe Celite was washed with ethyl acetate
  8. washthe filtrate was washed with saturated saline water
  9. dry with materialThe organic layer was dried with sodium sulfate
  10. customthe sodium sulfate was removed through filtration
  11. concentrationthe filtrate was concentrated under reduced pressure
  12. customthe residue was purified through silica gel column chromatography (hexane/ethyl acetate=100/0 to 85/15)