为改进5-甲基-6,7-二氢-5H-环戊并吡嗪(化合物2)的合成工艺条件,以甲基环戊烯醇酮和乙二胺为原料,无水乙醇作溶剂,二氧化锰作氧化剂,经缩合和氧化反应合成了化合物2,优化了合成条件,并采用1H NMR和IR技术对产物结构进行了表征。结果表明:当无水乙醇用量20 m L、n(甲基环戊烯醇酮)∶n(乙二胺)=1∶1.5(摩尔比)、60℃恒温反应2 h时,5-甲基-3,4,6,7-四氢-2H-环戊并吡嗪(化合物1)的收率达到95.7%;当n(氢氧化钾)∶n(二氧化锰)∶n(化合物1)=1∶2.4∶0.6、无水乙醇用量10 m L、80℃恒温反应15 h时,化合物2的收率为64.3%。
【英文摘要】
Cyclopenapyrazine compounds have important sensory properties in food and tobacco smoke. With anhydrous ethanol as solvent, manganese dioxide as oxidant, 5-methyl-6,7-dihydro-5H-cyclopentapyrazine(Compound 2) was synthesized by methyl cyclopentenolone and ethylenediamine via condensation cyclization and oxidation. Moreover, the synthesis conditions were optimized, and the structures of the products were characterized by1 H NMR and IR. The results showed that the yield of 5-methyl-3,4,6,7-tetrahydro-2H-cyclo...
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