HRID54027
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
To a solution of 1-bromo-2,6-dimethoxybenzene, (2.63 g, 12.1 mmol), tetrakis(triphenylphosphine)palladium (0) (0.91 g, 0.76 mol) and 1-naphthylboric acid (4.16 g, 23.9 mmol) in 1,4-dioxane (160 ml), a 2N aqueous solution of sodium hydroxide (13 ml) was added, and the mixture was heated to reflux. After cooling, the solvent was evaporated off, and the residue was dissolved in diethyl ether. The diethyl ether solution was washed with water and dried over anhydrous magnesium sulfate. Then, the solvent was evaporated off, and the residue was purified by silica gel column chromatography (developing phase: n-hexane/ethyl acetate=5/1) to obtain 1-naphthyl-2,6-dimethoxybenzene (2.50 g).
WORKUP
后处理
- temperaturethe mixture was heated to reflux
- temperatureAfter cooling
- customthe solvent was evaporated off
- dissolutionthe residue was dissolved in diethyl ether
- washThe diethyl ether solution was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- customThen, the solvent was evaporated off
- customthe residue was purified by silica gel column chromatography (developing phase: n-hexane/ethyl acetate=5/1)