| 钯催化的乙炔双羰化-高效合成丁烯二酸二甲酯 |
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| 引用本文： | 赵胜利,张勤生,马占伟,宋承立,裴晓平,熊绪茂,胡斌.钯催化的乙炔双羰化-高效合成丁烯二酸二甲酯[J].分子催化,2017,31(5):411-418. |
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| 作者姓名： | 赵胜利 张勤生 马占伟 宋承立 裴晓平 熊绪茂 胡斌 |
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| 作者单位： | 1. 中国科学院兰州化学物理研究所羰基合成与选择氧化国家重点实验室,甘肃兰州730000;中国科学院大学,北京100049;2. 中国科学院兰州化学物理研究所羰基合成与选择氧化国家重点实验室,甘肃兰州,730000 |
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| 基金项目： | 国家自然科学资金青年基金 |
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| 摘 要： | 报道了无酸和重金属盐的催化乙炔双羰化反应的钯催化体系(催化剂组成为PdCl2/KI).正交实验表明空气的初始分压和助剂KI的用量在乙炔双羰化反应中起着重要的作用.在相同的实验条件下,发现催化体系为PdCl2/HCl/CuCl2和PdCl2/H2SO4/FeCl3时,顺、反丁烯二酸二甲酯的总收率分别为15.3％和21.8％,而用PdCl/KI时总收率达到了81.9％.在最优反应条件下,即PdCl2 0.056 mmol,KI 0.677 mmol,总压5.3 MPa,70℃反应3h,顺、反丁烯二酸二甲酯的总收率为91.0％.
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| 关 键 词： | 钯催化 乙炔双羰化 马来酸二甲酯 碳-碳键形成 |
| 收稿时间： | 2017/8/28 0:00:00 |
| 修稿时间： | 2017/9/20 0:00:00 |
Palladium-catalyzed Dicarbonylation of Acetylene:Efficient Synthesis of Dicarboxylic Acid Dimethyl Esters |
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| ZHAO Sheng-li,ZHANG Qin-sheng,MA Zhan-wei,SONG Cheng-li,PEI Xiao-ping,XIONG Xu-mao and HU Bin.Palladium-catalyzed Dicarbonylation of Acetylene:Efficient Synthesis of Dicarboxylic Acid Dimethyl Esters[J].Journal of Molecular Catalysis (China),2017,31(5):411-418. |
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| Authors: | ZHAO Sheng-li ZHANG Qin-sheng MA Zhan-wei SONG Cheng-li PEI Xiao-ping XIONG Xu-mao and HU Bin |
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| Institution: | State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China;University of Chinese Academy of Sciences, Beij ing 100049, China,State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China,State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China,State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China,State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China;University of Chinese Academy of Sciences, Beij ing 100049, China,State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China and State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China |
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| Abstract: | In this work,we reported a palladium-catalyzed system (PdCl2/KI) without acid (HCl,H2SO4) and heavy metal salts cocatalyst (CuCl2 and FeCl3) for dicarbonylation of acetylene.The orthogonal experiments demonstrated that the partial pressure of air and the amounts of KI played the crucial roles in the reaction process.Moreover,comparison with other Pdcatalyzed systems (PdCl2/HCl/CuCl2,yield:15.3％ and PdCl2/H2SO4/FeCl3,yield:21.8％) under the same reaction conditions,the PdCl2/KI catalytic system showed much higher activity (yield:81.9％).The total yield of diesters can reach 91.0％ under the total pressure of 5.3 MPa with the catalyst composition of 0.056 mmol PdCl2 and 0.677 mmol KI at 70 ℃ for three hours. |
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| Keywords: | palladium catalyst dicarbonylation of acetylene diesters of maleic acid carbon-carbon bond-forming |
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