空气下Fe3O4@PDA-Pd NPs催化Heck反应制备3-苯基丙烯酸酯  

Preparation of 3-phenylacrylates through Heck reaction catalyzed by Fe3O4@PDA-Pd NPs under air atmosphere

作　　者：郭海昌 郑人华 蒋华江 赵丹味 徐振元[1] 夏爱宝[1] GUO Hai-chang;ZHENG Ren-hua;JIANG Hua-jiang;ZHAO Dan-wei;XU Zhen-yuan;XIA Ai-bao(Zhejiang Key Laboratory of Green Pesticides and Cleaner Production Technology,Zhejiang University of Technology,Hangzhou 310014,China;School of Pharmaceutical and Materials Engineering,Taizhou University,Taizhou 318000,China)

机构地区：[1]浙江工业大学浙江省绿色农药清洁生产技术研究重点实验室,浙江杭州310014 [2]台州学院医药化工与材料工程学院,浙江台州318000

出　　处：《高校化学工程学报》2020年第2期432-437,共6页Journal of Chemical Engineering of Chinese Universities

基　　金：浙江省自然科学基金(LY18B020017);浙江省公益技术研究计划(LGG19B040001);台州市科技计划项目(1801gy21)。

摘　　要：为研究在空气环境下经Heck反应制备3-苯基丙烯酸酯的合成方法,先在Fe3O4表面包裹聚多巴胺(PDA)形成Fe3O4@PDA亚微球,然后负载上纳米钯粒子(PdNPs)制备出Fe3O4@PDA-Pd NPs磁性复合物,再将该复合物用于催化卤代芳烃和丙烯酸酯的Heck反应,并对反应中的碱、溶剂、温度和催化剂用量等条件进行了优化。结果表明:催化剂用量为0.2%mol钯当量时,以三乙胺为碱,以N,N-二甲基甲酰胺为溶剂,80℃下反应3 h,碘代芳烃和丙烯酸酯经Heck反应制备3-苯基丙烯酸酯的收率大多在80%~90%;Fe3O4@PDA-PdNPs催化的Heck反应能在空气环境下进行,反应条件温和,对反应物取代基的耐受性好,催化剂分离简便。Fe3O4@PDA-Pd NPs magnetic composites were prepared by loading nano-Pd particles(Pd NPs)on Fe3O4@PDA submicrospheres formed by coating polydopamine(PDA)on Fe3O4 surface,which were used to catalyze the Heck reactions of aromatic halides and acrylate derivatives for the synthesis of 3-phenylacrylates under air atmosphere.The reaction conditions were optimized by studying the factors including alkali,solvent,temperature and catalyst dosage.The results show that the yields of 3-phenylacrylates were 80%~90%under the optimized conditions.The notable features of this method include wide availability of the substrates,compatibility with broad functional groups,mild conditions,simple catalyst separation and in particular it can be operated under air atmosphere.

关 键 词：四氧化三铁 HECK反应 纳米钯 3-苯基丙烯酸酯 

分 类 号：O611.62[理学—无机化学]