反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwere added to it
- customThe reaction liquid
- temperaturewas cooled to room temperature
- stirringstirred at room temperature
- customThe reaction liquid
- filtrationwas filtered through Celite
- washthe Celite was washed with ethyl acetate
- washthe filtrate was washed with saturated saline water
- dry with materialThe organic layer was dried with sodium sulfate
- customthe sodium sulfate was removed through filtration
- concentrationthe filtrate was concentrated under reduced pressure
- customthe residue was purified through silica gel column chromatography (hexane/ethyl acetate=100/0 to 85/15)