| 钯催化交叉偶联法合成7-乙炔基-2-芴基膦酸二乙酯 |
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| 引用本文： | 周舟,姚骏,毕峰,彭亮,潘晨晨,柳利,李法宝.钯催化交叉偶联法合成7-乙炔基-2-芴基膦酸二乙酯[J].湖北大学学报(自然科学版),2014(5):439-442. |
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| 作者姓名： | 周舟 姚骏 毕峰 彭亮 潘晨晨 柳利 李法宝 |
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| 作者单位： | 有机化工新材料湖北省协同创新中心(湖北大学),有机功能分子合成与应用教育部重点实验室湖北大学,湖北武汉430062 |
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| 基金项目： | 国家自然科学基金（21071049）和湖北省自然科学基金（2013CFA087）资助 |
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| 摘 要： | 以芴为原料,通过卤代、Sonogashira偶联、钯催化交叉偶联反应等合成了目标化合物7-乙炔基-2-芴基膦酸二乙酯.采用核磁共振谱(1 H、13 C、31P NMR)、傅里叶变换红外光谱(FT-IR)、液质联用飞行时间质谱(LC-MS TOF)等对目标化合物进行结构表征,表征数据与化合物结构相符.本文采用一步法直接合成膦酸酯,与传统的两步法相比,操作步骤更加简化,反应条件温和,避免使用五氯化磷、二氧化硫等毒性原料,钯催化交叉偶联反应产率高达91%.
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| 关 键 词： | 芴 炔 亚膦酸二乙酯 钯催化交叉偶联 合成 |
Synthesis of diethyl 7-ethynyl-2-fluorenylphosphonate via Pd-catalyzed cross-coupling method |
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| ZHOU Zhou,YAO Jun,BI Feng,PENG Liang,PAN Chenchen,LIU Li,LI Fabao.Synthesis of diethyl 7-ethynyl-2-fluorenylphosphonate via Pd-catalyzed cross-coupling method[J].Journal of Hubei University(Natural Science Edition),2014(5):439-442. |
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| Authors: | ZHOU Zhou YAO Jun BI Feng PENG Liang PAN Chenchen LIU Li LI Fabao |
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| Institution: | (Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials(Hubei University), Ministry of Education Key Laboratory for the Synthesis and Application of Organic Functional Molecules(Hubei University), Wuhan 430062, China) |
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| Abstract: | T his paper described the synthesis of the title compound diethyl 7-ethynyl-2-fluorenylphosphonate using fluorene as starting material by halogenation , Sonogashira coupling , palladium-catalyzed cross-coupling reactions .The structure of the title compound was characterized and confirmed by NMR （1H ,13C and 31P） ,FT-IR ,LC-MS TOF spectra .Compared with traditional two steps method , this method has advantages of one-step synthesis of aryl phosphonate , simplification of operation process , avoiding using poisonous PCl5 and SO2 , moderate reaction condition ,and the yield of Pd-catalyzed cross-coupling reaction as high as 91% . |
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| Keywords: | fluorene alkyne diethylphosphonate Pd-catalyzed cross-coupling synthesis |
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