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制备了1-磺酸丙基-3-甲基咪唑硫酸氢盐[MIMPS][HSO4]离子液体,以[MIMPS][HSO4]作为催化剂,应用于N2O5/有机溶剂硝化2,6-二乙酰氨基吡嗪-1-氧化物合成2,6-二氨基-3,5-二硝基吡嗪-1-氧化物(LLM-105)。通过1H NMR,IR和MS对LLM-105及其中间体的结构进行了表征。研究了在[MIMPS][HSO4]催化条件下,反应溶剂、催化剂用量、反应温度和反应时间对LLM-105收率的影响,结果表明最佳反应条件为:采用CH3NO2为反应溶剂,反应温度为55℃,反应时间为6 h,LLM-105的收率为72.2%。研究了[MIMPS][HSO4]的循环使用性能。结果表明,平行实验5次,平均收率71.7%,具有较好的可再生利用性。
The sulfonic acid propyl-3-methylimidazolium bisulfate [MIMPS] [HSO4] ionic liquid was prepared using [MIMPS] [HSO4] as a catalyst in the nitration of 2,6-diacetylamino Pyrazine-1-oxide 2,6-Diamino-3,5-dinitropyrazine-1-oxide (LLM-105). The structures of LLM-105 and its intermediates were characterized by 1H NMR, IR and MS. The effects of reaction solvent, amount of catalyst, reaction temperature and reaction time on the yield of LLM-105 were studied under [MIMPS] [HSO4] catalysis. The results showed that the optimal reaction conditions were: CH3NO2 as reaction solvent, 55 ℃, the reaction time was 6 h, the yield of LLM-105 was 72.2%. The cycling performance of [MIMPS] [HSO4] was studied. The results showed that the parallel experiment 5 times, the average yield of 71.7%, with good recyclability.