4-羟基-3-甲氧基苯乙酮肟环钯配合物催化Suzuki偶联反应的研究

Study on the Suzuki Coupling Reaction Catalyzed with 4-Hydroxy-3-methoxyacetophonene Oxime Palladiumcycle Complex

以4-羟基-3甲氧基苯乙酮为原料,通过肟化反应合成了4-羟基-3甲氧基苯乙酮肟,并以氯钯酸锂为钯源,合成了4-羟基-3-甲氧基苯乙酮肟环钯配合物.通过傅立叶红外(FT-IR)和紫外-可见漫反射光谱(UV-vis-DRS)对合成的配合物进行了表征.考察了溶剂与溶剂含水量、碱、催化剂用量等反应条件对4-羟基-3甲氧基苯乙酮肟环钯配合物催化Suzuki偶联反应的影响.当以碳酸钾为碱,乙醇水溶液(50vol%)为溶剂,催化剂量为0.01%(1×10^-4mmol),60℃下催化对溴苯乙酮与苯硼酸Suzuki偶联反应,反应15min时,产品收率可达98.76%,表明4-羟基-3-甲氧基苯乙酮肟环钯配合物催化剂具有很高的催化效率.

The 4-hydroxy-3-methoxyacetophonene oxime is synthesized from 4-hydroxy-3-methoxyacetophonene by the oximation reaction and the 4-hydroxy-3-methoxyacetophenone oxime palladiumcycle complex is prepared with the lithium palladium chloride as palladium source.The asprepared complex is characterized by Fourier transform infrared spectroscopy(FT-IR)and UV-visible diffuse reflection spectrum(UV-vis-DRS).The effects of reaction conditions,such as solvent,water content,alkali,catalyst adding amount on the Suzuki coupling reaction catalyzed with 4-hydroxyl-3-methoxyacetophenone oxime palladiumcycle complex are investigated.When the Suzuki coupling reaction between p-bromine acetophenone with phenylboronic acid is carried out at 60℃ with K2 CO3 as alkali,ethanol aqueous solution(50 vol%)as solvent,catalyst adding amount of 0.01%(1×10-4 mmol),the yield can reach 98.76% in 15 min.The results show that 4-hydroxy-3-methoxyacetophenone oxime palladiumcycle complex catalyst has high catalytic efficiency.