HRID1061883
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
A mixture of 6-bromo-1-formyl-2-naphthyl trifluoromethanesulfonate (5.62 g), triethylamine (5.12 mL), methanol (10 mL), palladium acetate (0.20 g), 1,1′-bis(diphenylphosphino)ferrocene (0.49 g) and DMF (30 mL) was stirred under a carbon monoxide atmosphere at room temperature for 3 hrs. The reaction mixture was diluted with ethyl acetate and washed successively with 10% citric acid, water and saturated aqueous sodium hydrogen carbonate, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography (carrier: silica gel, developing solvent: hexane-ethyl acetate, 20:1-3:1) to give the title compound (1.66 g) as colorless crystals.
WORKUP
后处理
- washwashed successively with 10% citric acid, water and saturated aqueous sodium hydrogen carbonate
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
- customThe residue was purified by column chromatography (carrier: silica gel, developing solvent: hexane-ethyl acetate, 20:1-3:1)