1,4-二硝基呋咱并[3,4-b]哌嗪(DNFP)的合成  

Synthesis of 1,4-Dinitrofurazano[3,4-b] piperazine(DNFP)

作　　者：毕福强[1] 王伯周[1] 王锡杰[1] 熊存良[1] 贾思媛[1] 

机构地区：[1]西安近代化学研究所,陕西西安710065

出　　处：《含能材料》2009年第5期537-540,共4页Chinese Journal of Energetic Materials

基　　金：国家重点基础研究发展计划子专题(No.613740102)

摘　　要：设计合成了高能量密度材料1,4-二硝基呋咱并[3,4-b]哌嗪(DNFP)。即以N,N′-二叔丁基乙二胺为起始原料,低温条件下与二氯乙二肟缩合环化生成1,4-二叔丁基哌嗪-2,3-二酮肟(PDO-tB),而后在氢氧化钠的乙二醇溶液中高温反应脱水环化得1,4-二叔丁基呋咱并[3,4-b]哌嗪,经98%硝酸和硫酸的混酸体系硝解合成出DNFP,总收率32.6%,采用红外光谱、核磁共振谱、元素分析对DNFP和中间体结构进行了表征;改进了PDO-tB的合成工艺条件,加料方式由一次性加入改为缓慢滴加,并确定了适宜的冷浴温度为-18℃;研究了不同硝解体系对反应的影响,确定了适宜的硝解体系为硝硫混酸,硝解收率为61.7%。The synthesis of 1,4-dinitrofurazano[ 3,4-hi piperazine （DNFP） with an overall yield of 32.6%, was described. The eyelizative condensation between N, N＇-di-tert-butyl ethylenediamine and diehloroglyoxime at low temperature generated 1,4-di-tert-butyl piperazine-2,3-dioxime （PDO-tB）, whieh underwent a base-promoted dehydration at high temperature to obtain 1,4-di-tert-butylfurazano[3,4-b] piperazine （FP-tB）. Furthermore, nitrolysis of FP-tB provided an efficient access to the novel explosive compound DNFP. The structures of DNFP and its intermediates were characterized by IR, ^1H NMR, ^13C NMR and elemental analysis. Moreover, the effects of reaction conditions on the yield of PDO-tB were studied, and the optimum reaction condition is dropwise addition at - 18 ℃. Converting FP-tB to DNFP with several nitrolysis reagents were also studied,and the nitrolysis with the mixed acid of 98% HNO3 and H2SO4 provides a good yield of 61.7%.

关 键 词：有机化学 1 4-二硝基呋咱并[3 4-b]哌嗪(DNFP) 呋咱 哌嗪 合成 表征 

分 类 号：TQ564[化学工程—炸药化工]