[MIMPS][HSO_4]催化N_2O_5硝化2,6-二乙酰氨基吡嗪-1-氧化物

Nitration of 2,6-Diacetamidopyrazine-1-oxide with N_2O_5 Catalyzed by [MIMPS][HSO_4]

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。

Ionic liquid 1-sulfonicacidpropyl-3-methylimidazole hydrosulfate [ MIMPS] [ HSO4 ] was prepared as a catalyst to synthesize 2,6-diamino-3,5- dinitropyrazine-l-oxide （ LLM-105 ） from nitration of 2,6-diacetamido-pyrazine-1-oxide with N20s/solvents. The structures of intermediates and LLM-105 were determined by ^1H NMR, IR and MS. The effects of reaction solvents, amount of [MIMPS] [HSO4] ,reaction temperature,reaction time and repeated use of [MIMPS] [ HSO4] on the yield of LLM-105 were studied. Results show that the optimized reaction conditions are： CH3 NO2 as solvent; reaction temperature 55 ℃;reaction time 6 h. The yield of LLM-105 is 72.2%. The ionic liquid is suitable for repetition use.