Pd(Ⅱ)-salen配合物的制备及水相催化Suzuki反应  

Preparation of Pd(Ⅱ)-Salen Complex and Its Application as an Efficient Catalyst for Suzuki Reaction in Water

作　　者：鄢仲钰 何静远 史大斌 YAN Zhong-yu;HE Jing-yuan;SHI Da-bin(Key Laboratory of Biocatalysis&Chiral Drug Synthesis of Guizhou Province,School of Pharmacy,Zunyi Medical University,Zunyi 563000,China)

机构地区：[1]遵义医科大学药学院贵州省生物催化与手性药物合成重点实验室,贵州遵义563000

出　　处：《化学试剂》2021年第12期1749-1754,共6页Chemical Reagents

基　　金：国家自然科学基金资助项目(21362047,21861045);遵义医科大学大学生创新训练计划资助项目(ZYDC2020038)。

摘　　要：以4-羟基-3-甲氧基苯甲酸为起始原料,经Duff反应、缩合和配位等反应步骤,合成了一个新型含羧基的Pd(Ⅱ)-salen催化剂,该催化剂能溶于碱性水溶液中并在水溶液中有效催化溴代芳烃与芳基硼酸发生Suzuki偶联反应,反应使用0.5 mol%催化剂,水为溶剂,空气环境中90℃反应24 h,以良好产率生成联芳基化合物。合成的催化剂及偶联产物的结构经NMR和HRMS确证。实验结果表明,该催化反应在水相中进行,无需膦配体且水相能循环使用3次,具有操作方便及环境友好的特点。A new Pd(Ⅱ)-salen complex I containing carboxylic acid groups was synthesized from 4-hydroxy-3-methoxybenzoic acid by the Duff reaction,condensation,and coordination.Compound I can be dissolved in an alkaline water solution and effectively catalyze the Suzuki coupling of aryl bromides and arylboronic acids in aqueous medium to produce biaryl compounds in good yields.The structures of biaryls were confirmed by NMR and HRMS analysis.The experimental results showed that the reaction was processed in the aqueous phase without phosphine ligand,and the aqueous phase was reused three times for the Suzuki reaction.This protocol provides several advantages such as simple operation and environment friendly.

关 键 词：绿色化学 Pd(Ⅱ)-salen配合物 SUZUKI偶联反应 联芳基化合物 水相 

分 类 号：O621.3[理学—有机化学]