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机构地区:[1]郑州大学化学系,郑州450052
出 处:《应用化学》2005年第5期494-497,共4页Chinese Journal of Applied Chemistry
基 金:河南省自然科学基金资助项目(0111030900)
摘 要:水杨醛与壳聚糖反应制得壳聚糖席夫碱配体,再与钯盐反应得到壳聚糖席夫碱钯催化剂。以碘代苯(PhI)与丙烯酸(AA)偶联生成肉桂酸为模型反应,研究了该催化剂的催化性能。考察了不同反应条件(反应温度、原料比、催化剂用量、缚酸剂种类及用量、溶剂)对该反应的影响,由此确定了该催化反应的最佳反应条件:PhI10mmol,n(PhI)∶n(AA)=1∶1.5,三乙胺用量27mmol,催化剂0.1g(Pd质量分数为2%),以DMF为溶剂,N2气保护下70℃反应7h,产率达90.7%。该催化剂经过滤分离、溶剂洗涤,重复使用6次仍有较高的催化活性。Chitosan schiff-base was synthesized via the reaction of chitosan with salicylaldehyde, which (reacted) with a palladium salt to obtain a chitosan schiff-base coordinated palladium catalyst. Using the reaction between iodobenzene and acrylic acid as a model, we studied the activity of this catalyst. The effects of (different) reaction conditions (reaction temperature, molar ratio of iodobenzene to acrylic acid, catalyst (loading), kind and quantity of base and solvent) on the yield were investigated. The best conditions for the (reaction) were established as PhI 10mmol; n(PhI)∶n(AA)=1∶1.5; Et_(3)N 27 mmol; catalyst(mass (fraction) 2%) 0.1 g; solvent DMF 6 mL; 70 ℃ for 7 h. Under the above best conditions, the yield was 90.7%. The catalyst was separated from the reaction mixture via filtration washed with solvent, and then reused. After 6 cycles no significant loss of catalyst activity was observed.
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