微波辅助合成1-甲基-2,4,5-三碘基咪唑

摘要

2,4,5-triiodo-1-methylimidazole was synthesized using N-methylimidazole as starting material via iodination of I 2/HIO 3 acidic solution under microwave irradiation. The infrared spectra analysis, elemental analysis and high performance liquid chromatography(HPLC) were adopted for product characterization and purity determination. The effects of reaction time, reaction temperature, the quality of iodine and iodic acid on the iodo-reaction results were studied. The results showed that the optimum parameters of iodination process are reaction time of 60min,reaction temperature of 80℃,n(iodine):n(iodic acid):n(N-methylimidazole)=2:3:1. HPLC analysis showed the purity of MTII was over 98%.%在微波加热条件下，以N-甲基咪唑为原料，用I2/HIO3的酸性溶液碘化合成1-甲基-2,4,5-三碘基咪唑（MTII）。采用红外光谱、元素分析和高效液相色谱等方法对合成产物MTII进行了结构表征和纯度分析，讨论了反应温度、反应时间、碘、碘酸用量对碘代反应的影响。结果表明，碘代反应的最佳反应条件为：反应温度80℃，反应时间60min，n （I2）：n （HIO3）∶n （C4H6N2）=2∶3∶1，高效液相色谱分析表明MTII纯度大于98％。