CAJ | 학술논문

以3，5-二硝基吡唑为原料，三甲基苯磺酰羟胺（ MSH）为胺化剂，合成了1-氨基-3，5-二硝基吡唑（ ADNP），收率60．7％。用 IR、1 H NMR、13 C NMR、MS 和元素分析表征了其结构。在乙醇中培养了单晶。用四圆 X 射线衍射仪测定了它的单晶结构：ADNP属正交晶系，P2（1）/n 空间群，a ＝5．543（2）？，b ＝9．866（4）？，c ＝11．745（5）？，Z ＝4，D c ＝1．79 g·cm -3。DSC 结果表明，两个吸热峰温度分别为110℃和264℃；TG 结果表明，在170～268℃之间为急剧失重过程，失重99．1％。
이3，5-이초기필서위원료，삼갑기분광선간알（ MSH）위알화제，합성료1-안기-3，5-이초기필서（ ADNP），수솔60．7％。용 IR、1 H NMR、13 C NMR、MS 화원소분석표정료기결구。재을순중배양료단정。용사원 X 사선연사의측정료타적단정결구：ADNP속정교정계，P2（1）/n 공간군，a ＝5．543（2）？，b ＝9．866（4）？，c ＝11．745（5）？，Z ＝4，D c ＝1．79 g·cm -3。DSC 결과표명，량개흡열봉온도분별위110℃화264℃；TG 결과표명，재170～268℃지간위급극실중과정，실중99．1％。
1-Amino-3,5-dinitropyrazole(ADNP)was synthesized using 3,5-dinitropyrazole as raw material and 2,4,6-trimethyl-benzenesulfonic hydroxylamine(MSH)as aminating agent with a yield of 60. 7% . Its structure was characterized by IR,NMR, MS and element analyses. The single crystal was cultivated in ethanol. Its single crystal structure was determined by a four-circle X-ray diffractometer. Its thermal properties were studied by TG-DSC. Results show that the crystal is orthorhombic,space group P2(1)/n with crystal parameters of a =5. 543(2)?,b =9. 866(4)?,c =11. 745(5)?,Z =4,D c =1. 79 g·cm -3 ,V =642. 3(4)?3 . Thermal analyses demonstrate that there is a sharp mass loss process from 170 ℃ to 266 ℃ with 99. 1% mass loss. The two endo-thermic peaks temperatures appear at 110 ℃ and 264 ℃.