【摘要】 以硝基甲烷为原料,低温氧化硝化制得2,2-二硝基-1,3-丙二醇,银回收率达93%以上,并成功实施了循环使用。2,2-二硝基-1,3-丙二醇经一锅法制得2,2-二硝基乙醇钾,收率达62%以上(文献值约52%);再在68%的硝酸中进行环化,在50~60℃时首先得到三硝基吡啶N-氧化物(TNPyO),继续升温至80~90℃回流1 h,制得三硝基吡啶(TNPy),二者产率分别为50%和15%。改用磷酸和硫酸也可以得到化合物TNPyO。产物经红外光谱、核磁共振、元素分析和质谱等进行了表征。更多还原

【Abstract】 2,2-Dinitropropane-1,3-diol was synthesized from nitromethane in low temperature by oxidative nitration method.Silver was successfully recycled with a yield upon 93% and reused in the synthesis of 2,2-dinitropropane-1,3-diol.Potassium 2,2-dinitroethanol,the key intermediatecompound for synthesis of trinitropyridine(TNPy),was prepared through one-pot method with a yield upon 62%,which is 10% higher than conventional method.Controlling the pH value in the range of 1-2,trinitropyridine N-oxide(TNPyO) was synthesized by the cyclization of potassium 2,2-dinitroethanol in 68% nitric acid at 50-60℃.Maintaining the temperature between 80-90 ℃,TNPyO can be further reduced to produce TNPy by refluxing for 1 h;The yields of TNPyO and TNPy are 50% and 15%,respectively.TNPyO can also be prepared from potassium 2,2dinitroethanol under phosphoric acid and sulfuric acid.The products were characterized by IR,nuclear magnetic resonance,elemental analysis and EI-MS.更多还原