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菲啰啉吡咯的合成工艺改进

Process Improvement on the Synthesis of Phenanthrolinopyrrole
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摘要 1,10-邻菲啰啉经硝化反应制得5-硝基-1,10-邻菲啰啉(1)。以无水乙醇为溶剂,1与异氰基乙酸乙酯在K2CO3的催化下通过Barton-Zardon反应合成了一种稠合菲啰啉环并吡咯衍生物2。较佳的反应条件为:1 10mmol,n(1)∶n(异氰基乙酸乙酯)∶n(K2CO3)=1.0∶1.0∶1.1,于室温反应24 h,产率59.3%。 5-Nitro-1,10-phenanthroline(1) was prepared by nitration of 1,10-phenanthroline with concentrated nitric acid and concentrated sulfuric acid.A kind of pyrrole derivative fused with phenanthroline ring(2) was synthesized by Barton-Zardon reaction of 1 with ethyl isocyanoacetate in the presence of K2CO3 using in dry ethanol as the solvent.The optimum reaction conditions at room temperature for 24 h were as followes: 1 was 10 mmol,n(1) ∶ n(ethyl isocyanoacetate) ∶ n(K2CO3)=1.0 ∶ 1.0 ∶ 1.1.The yield of 2 was 59.3% under the optimum conditions.
出处 《合成化学》 CAS CSCD 北大核心 2011年第2期261-263,共3页 Chinese Journal of Synthetic Chemistry
基金 河南省科技厅科技攻关项目(082102210050) 河南省教育厅自然科学研究计划项目(2008B150018) 安徽省高等学校科研项目(KJ2007B093) 2010年商丘师范学院青年骨干教师计划项目
关键词 5-硝基-1 10-邻菲啰啉 Barton-Zard反应 菲啰啉吡咯 工艺改进 合成 5-nitro-1 10-phenanthroline Barton-Zard reaction phenanthrolinopyrrole process improvement synthesis
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参考文献11

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