4,10-二硝基-2,6,8,12-四氧杂-4,10-二氮杂四环5.5.0.0<sup>5,9</sup>0<sup>3,11</sup>十二烷的合成

4,10-二硝基-2,6,8,12-四氧杂-4,10-二氮杂四环5.5.0.0^5,90^3,11十二烷的合成

摘要: 研究了4,10-二硝基-2,6,8,12-四氧杂-4,10-二氮杂四环5.5.0.0^5,90^3,11十二烷(TEX)的合成方法,以其二步合成法为基础,对影响中间体1, 4-二甲醛-2, 3, 5, 6-四羟基哌嗪(DFTHP)以及目标产物4,10-二硝基-2,6,8,12-四氧杂-4,10-二氮杂四环5,5,0,0^5,90^3,11十二烷(TEX)合成收率的关键因素进行了考察. 结果表明:使用NaOH饱和溶液调节反应液pH为9时,DFTHP收率可达到68.3%;硝硫混酸中发烟硝酸与浓硫酸的体积比为3∶2,硝化剂与DFTHP的体积与质量比为3∶1时TEX的收率可达到59.7%. 经过条件优化,TEX二步合成法总收率提高到了40.8%.

Abstract: This paper studies two-step synthetic process of TEX (4,10-dinitro-2,6, 8,12-tetraoxa-4, 10-diazatetracyclo-5.5.0.0^5,90^3,11-dodecane) and the effects of key factors on the yield of DFTHP (intermediate) and TEX. The results show that the yield of DFTHP could reach to 68.3% when the adjusted pH value of reaction solution reaches to 9 by saturated NaOH solution. When the volume ratio of fuming HNO₃ to concentrated H₂SO₄ is 3∶2, and the ratio of nitrating agent (mL) to DFTHP(g) is 3:1, the yield of TEX raises to 59.7% . The optimized overall yield of TEX obtained from two-step synthetic process could be 40.8%.