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
PROCEDURE
实验过程
Under an argon atmosphere, 170 g of the resulting 1-bromo-4-(2-formylphenyl)naphthalene, 207 g of methoxymethyl triphenylphosphonium chloride and 2.0 L of tetrahydrofuran (THF) were placed in a flask. During stirring at room temperature, 73.6 g of potassium t-butoxide was added to the flask. After further stirring at room temperature for 2 hours, 1.5 L of water was added. The reaction solution was extracted with diethyl ether. An aqueous phase was removed and 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 180 g (yield: 99%) of 1-bromo-4-[1-(2-methoxyvinyl)phenyl]naphthalene was obtained.
WORKUP
后处理
- stirringAfter further stirring at room temperature for 2 hours
- extractionThe reaction solution was extracted with diethyl ether
- customAn aqueous phase was removed
- customan organic phase which had been separated
- washwas washed with water and saturated brine
- dry with materialdried with magnesium sulfate
- filtrationAfter the magnesium sulfate was filtered out
- concentrationthe organic phase was concentrated
- customThe resulting residue was purified by means of silica gel column chromatography