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采用浸渍-还原法制备三氧化二铝负载钯催化剂(Pd/Al2O3),通过ICP-AES、XRD、XPS等分析手段对催化剂的结构和组成进行了表征。考察了溶剂、溶剂与水的比例、碱的种类、反应温度以及反应时间等反应条件对上述制备的催化剂催化Suzuki偶联反应的影响,筛选出最适宜的反应条件。实验结果表明,在1mmol对溴苯乙酮,1.5mmol苯硼酸,2mmol碳酸钾,乙醇∶水=6∶6,反应温度为60℃,反应时间为60min,催化剂加入量为3.5×10-3mmol钯的反应条件下,Suzuki反应收率可达97%以上。
The supported alumina catalyst (Pd / Al2O3) was prepared by impregnation-reduction method. The structure and composition of the catalyst were characterized by ICP-AES, XRD and XPS. The effects of reaction conditions such as solvent, solvent to water ratio, type of base, reaction temperature and reaction time on the catalytic Suzuki coupling reaction were investigated. The optimum reaction conditions were screened out. The experimental results show that when the amount of catalyst is 3.5 × 10-3mmol, the reaction time is 60min at 1mmol of p-bromoacetophenone, 1.5mmol of phenylboronic acid, 2mmol of potassium carbonate, ethanol: water = 6: 6, the reaction temperature is 60 ℃, Under the reaction conditions, the Suzuki reaction yield up to 97%.