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作 者:高银红 秦山林 孙佳烽 郭艺伟 张强 Gao Yinhong;Qin Shanlin;Sun Jiafeng;Guo Yiwei;Zhang Qiang(Tianping College of Suzhou University of Science and Technology,Suzhou 215009,China;School of Chemistry,Biology and Material Engineering,Suzhou University of Science and Technology,Suzhou 215009,China)
机构地区:[1]苏州科技大学天平学院,江苏苏州215009 [2]苏州科技大学化学生物与材料工程学院,江苏苏州215009
出 处:《山东化工》2018年第12期13-15,共3页Shandong Chemical Industry
基 金:江苏省高等学校大学生创新创业训练计划项目(201713985010Y;201710332051X);江苏省自然科学基金(BK20150282)
摘 要:研究了一种磁性纳米钯催化廉价的邻氯苯腈与对甲基苯硼酸Suzuki偶联合成沙坦联苯的新方法。目标产物经熔点、红外、核磁及质谱表征。考察了溶剂、温度、催化剂用量及反应时间的影响,确定了最佳的反应条件。邻氯苯腈2.0 mmol,对甲基苯硼酸2.2 mmol,碳酸钾4.0 mmol,四丁基溴化铵0.2 mmol,钯催化剂1.0 mol%,DMF 20 m L,110℃反应12 h,产率可达92%。此外,催化剂经简单磁分离即可高效回收,重复使用4次,活性无明显下降。A novel method for the synthesis of sartanbiphenyl via the Suzuki coupling with 2-chlorobenzonitrile and 4-tolylboronic acid by the magnetic nano-palladium catalyst was reported.The target product was characterized by melt point,FTIR,1H NMR and MS.The effects of solvent,temperature,usage of catalyst and time on the reaction were investigated and the best reaction conditions were obtained.The mixture of 2-chlorobenzonitrile(2.0 mmol),4-tolylboronic acid(2.2 mmol),K 2CO 3(4.0 mmol),TBAB(0.2 mmol),MNP-Pd(1.0 mol%)and DMF(20 mL)were reacted at 110℃for 12 h,which afforded 92%yield.Moreover,the catalyst could be efficiently recycled by the simple magnetic separation and it could be reused 4 times without a significant loss of catalytic activity.
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