| 氮杂环卡宾-钯功能化的配位聚合物（NHC-Pd@Zn-L）：合成、表征及催化Suzuki-Miyaura交叉偶联反应 |
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| 引用本文： | 郭杰,张帆,谢世玉,由立新,孙亚光. 氮杂环卡宾-钯功能化的配位聚合物（NHC-Pd@Zn-L）：合成、表征及催化Suzuki-Miyaura交叉偶联反应[J]. 化工学报, 2022, 73(8): 3608-3614. DOI: 10.11949/0438-1157.20220233 |
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| 作者姓名： | 郭杰 张帆 谢世玉 由立新 孙亚光 |
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| 作者单位： | 沈阳化工大学理学院,辽宁 沈阳 110142 |
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| 基金项目： | 辽宁省教育厅科学研究经费项目(LJKZ0432);国家自然科学基金面上项目(21671139) |
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| 摘 要： | 以-二(1-羧乙基)咪唑盐(HL)和Zn(NO3)2·6H2O反应合成二维配位聚合物[Zn(L)2] n (Zn-L),产物再与K2PdCl4在四氢呋喃溶液中反应引入氮杂环卡宾-钯（NHC-Pd）催化位点,制得催化剂NHC-Pd@Zn-L,并通过PXRD、TGA、ICP、SEM、EDS和XPS进行表征。结果表明,NHC-Pd@Zn-L具有良好的热稳定性且修饰后晶体的框架结构没有发生变化,Pd以NHC-Pd的形式结合在Zn-L中,并均匀分散在配位聚合物中。将NHC-Pd@Zn-L用于催化Suzuki-Miyaura交叉偶联反应,当以苯硼酸和溴苯为底物,催化剂用量为15 mg,乙醇为溶剂,碳酸钾为碱的条件下60℃反应6 h,产率达到>99%,而且催化剂易于回收并可循环使用3次。
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| 关 键 词： | 氮杂环卡宾-钯 Suzuki-Miyaura交叉偶联反应 催化 配位聚合物 后合成修饰 |
| 收稿时间： | 2022-02-23 |
NHC-Pd functionalized coordination polymer (NHC-Pd@Zn-L): synthesis,characterization and catalytic performance in Suzuki-Miyaura cross-coupling reaction |
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| Jie GUO,Fan ZHANG,Shiyu XIE,Lixin YOU,Yaguang SUN. NHC-Pd functionalized coordination polymer (NHC-Pd@Zn-L): synthesis,characterization and catalytic performance in Suzuki-Miyaura cross-coupling reaction[J]. Journal of Chemical Industry and Engineering(China), 2022, 73(8): 3608-3614. DOI: 10.11949/0438-1157.20220233 |
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| Authors: | Jie GUO Fan ZHANG Shiyu XIE Lixin YOU Yaguang SUN |
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| Affiliation: | College of Science, Shenyang University of Chemical Technology, Shenyang 110142, Liaoning, China |
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| Abstract: | A two-dimensional coordination polymer [Zn(L)2] n(Zn-L) was synthesized by the reaction of 1,3-bis(1-carboxyethyl) imidazolium salt (HL) and Zn(NO3)2·6H2O. The product was then reacted with K2PdCl4 in tetrahydrofuran solution to introduce nitrogen heterocyclic carbene-palladium (NHC-Pd) catalytic site to prepare the catalyst NHC-Pd@Zn-L, and the structure was characterized by PXRD, TGA, ICP, SEM, EDS and XPS. The results showed that the catalyst had high thermal stability and the framework structure of the modified Zn-L did not change, and Pd was bound in Zn-L in the form of NHC-Pd and uniformly dispersed in the coordination polymer. NHC-Pd@Zn-L was used to catalyze the Suzuki-Miyaura cross-coupling reaction. When phenylboronic acid and bromobenzene were used as substrates, the catalyst dosage was 15 mg, ethanol was used as solvent, and potassium carbonate was used as base for the reaction at 60℃, 6 h, the yield reaches >99%, and the catalyst is easy to recover and can be recycled for 3 times. |
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| Keywords: | N-heterocyclic carbine-Pd Suzuki-Miyaura cross-coupling reaction catalysis coordination polymer post-synthetic modification |
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