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出 处:《化学研究与应用》2015年第4期497-500,共4页Chemical Research and Application
摘 要:本文以3-甲基-4-硝基氮氧化吡啶为起始原料,经两步反应合成5-氮杂吲哚。通过单因素实验法研究了温度、N,N-二甲基甲酰胺(DMF)、N,N-二甲基甲酰胺二甲缩醛(DMA)、铁粉等因素对反应的影响。较佳工艺条件下,产品按3-甲基-4-硝基吡啶氮氧化物计总收率为88.57%,较文献[1,2]提高了6%。通过熔点测定、1H NMR对最终产物进行了结构表征。此工艺的优点在于操作简单,反应时间短,成本低,收率高,适合于工业化生产。The 5-aza-indole was synthesized two-step with 3-methyl-4-nitro-pyridine nitrogen oxide as the starting material. Through single factor experiment,the effect of the amount of N,N-dimethylformamide,N,N-dimethylformamide dimethylacetal,iron and other factors on the yields were investigated. Under the best operational conditions,the yield was 88. 57%,much better than the reported value 82%. The melting point of the product was measured,and the structure of the compound was characterized by1H-NMR. The advantage of this process was that simple operation,short reaction time,low cost,high yield,suitable for industrial production.
关 键 词:3-甲基-4-硝基吡啶氮氧化物 5-氮杂吲哚 合成
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