TMPSHSO_4催化N_2O_5/有机溶剂硝化2,6-二乙酰氨基吡啶-1-氧化物

Nitration of 2,6-Diacetamidopyridine -1-oxide with N_2O_5/Solvents Catalyzed by TMPSHSO_4

以2,6-二乙酰氨基吡啶-1-氧化物(DAPO)为原料,在N,N,N-三甲基-N-丙磺酸基-硫酸氢铵(TMPSHSO4)催化条件下,采用N2O5/有机溶剂硝化2,6-二乙酰氨基吡啶制得2,6-二氨基-3,5-二硝基吡啶-1-氧化物(ANPyO)。考察了在TMPSHSO4催化条件下反应溶剂、温度和时间对ANPyO产率的影响,结果表明最佳反应条件为:反应溶剂为CH3NO2,反应温度为60℃,反应时间为5h,ANPyO产率为92.5%。用1H NMR,IR和MS对ANPyO的结构进行了表征。

2,6-Diamino-3,5-dinitropyridine-1-oxide （ ANPyO ） was synthesized from nitration of 2,6-diaeetamidopyridine-1-oxide （DAPO） with N2O5/solvents and N,N,N-trimethyl-N-propanesulfonic acid ammonium hydrogen sulfate （TMPSHSO4 ） as the nitrating agent and eatalyst. The effects of reaction solvent,temperature and time on the yield of ANPyO were studied. The optimal reaction conditions were obtained： reaetion solvent is CH3 NO2 ; reaction temperature is 60 ℃; reaction time is 5 h ; the yield of product is 92.5%. The structure of ANPyO were characterized by ^1H NMR,IR and MS.