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 7-(trifluoromethanesulfoxy)-1-tetralone (23.3 g), phenyl borate (11.8 g), potassium carbonate (21.9 g), toluene (500 ml), ethanol (50 ml) and water (50 ml) was stirred for 30 minutes at room temperature under argon atmosphere, and to the mixture was added tetrakis(triphenylphosphine)palladium (3.66 g). The mixture was refluxed for 20 hours and then cooled to room temperature. The organic layer was separated, washed with saturated sodium chloride solution, dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was separated and purified with column chromatography (ethyl acetate/toluene/hexane=1/5/5) to give 7-phenyl-1-tetralone (15.1 g) as pale brown oil.
WORKUP
后处理
- temperatureThe mixture was refluxed for 20 hours
- temperaturecooled to room temperature
- customThe organic layer was separated
- washwashed with saturated sodium chloride solution
- dry with materialdried with anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was separated
- custompurified with column chromatography (ethyl acetate/toluene/hexane=1/5/5)