| 磷钨酸铝催化合成9-苯甲酰蒽 |
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| 引用本文： | 陈敏,黄立静,李培仙,李国芳,谢吉民,袁新华.磷钨酸铝催化合成9-苯甲酰蒽[J].精细化工,2008,25(12). |
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| 作者姓名： | 陈敏 黄立静 李培仙 李国芳 谢吉民 袁新华 |
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| 作者单位： | 江苏大学,化学化工学院,化学系,江苏,镇江,212013;江苏大学,材料科学与工程学院,材料科学系,江苏,镇江,212013 |
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| 基金项目： | 国家自然科学基金
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江苏大学高级人才科研启动基金
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| 摘 要： | 为合成功能高分子中间体9-苯甲酰蒽,考察了以杂多酸型催化剂磷钨酸铝(AlPW12O40)催化蒽和苯甲酰氯的Friedel-Crafts酰基化反应,提纯得到w(9-苯甲酰蒽)=96.3,用GC/MS、FTIR和1HNMR等确认了其结构;考察了各反应条件对9-苯甲酰蒽产率和选择性的影响,得到9-苯甲酰蒽的优化合成条件为:反应温度90℃,反应时间5h,n(蒽):n(苯甲酰氯)=1.0:1.5,w(催化剂)=4.5,溶剂为环己烷。在上述条件下,9-苯甲酰蒽的产率和选择性分别可达47.4和91.8。证明AlPWO对目标产物选择性高、无环境污染,可以回收利用。
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| 关 键 词： | 磷钨酸铝 9-苯甲酰蒽 酰基化 蒽 苯甲酰氯 精细化工中间体 |
Synthesis of 9-Benzoylanthracene Catalyzed by AlPW12O40 Heteropolyacid |
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| CHEN Min,HUANG Li-jing,LI Pei-xian,LI Guo-fang,XIE Ji-min,YUAN Xin-hua.Synthesis of 9-Benzoylanthracene Catalyzed by AlPW12O40 Heteropolyacid[J].Fine Chemicals,2008,25(12). |
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| Authors: | CHEN Min HUANG Li-jing LI Pei-xian LI Guo-fang XIE Ji-min YUAN Xin-hua |
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| Abstract: | 9-Benzoylanthracene was prepared via Friedel-Crafts acylation of anthracene with benzoyl chloride catalysed by AlPW12O40 heteropolyacid.The structure of 9-benzoylanthracene was confirmed by GC/MS,FTIR and 1HNMR.The most suitable synthesis conditions are:cyclohexane as solvent,n(benzoyl chloride)∶n(anthracene)=2∶1,catalyst mass fraction 4.5%,reaction temperature 90 ℃ and reaction time 5 h.Yield of 9-benzoylanthracene is 47.4% and the selectivity for 9-benzoylanthracene is 91.8%.Purity of the refined product is w(benzoylanthracene)=96.3%.Additionally,AlPW12O40 has no pollution to environment and can be easily recovered for reuse. |
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| Keywords: | AlPW12O40 heteropolyacid 9-benzoylanthracene acylation anthracene benzoyl chloride fine chemical intermediates |
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