2,6-二氨基-3,5-二硝基吡啶的制备及表征  

Preparation and Characterization of 2,6-Diamino-3,5-dinitropyridine (DADNP)

作　　者：王艳红[1] 黄玉东[1] 宋元军[1] 胡桢[1] 孟祥丽[1] 景介辉[1] 

机构地区：[1]哈尔滨工业大学应用化学系,黑龙江哈尔滨150001

出　　处：《化学与粘合》2009年第5期4-6,共3页Chemistry and Adhesion

基　　金："863"高科技计划项目(编号:2002AA305109);航天创新科技基金(编号:24409035)

摘　　要：为制备高纯度高收率的2,6-二氨基-3,5-二硝基吡啶(DADNP),我们以2,6-二氨基吡啶(DAP)为原料,采用发烟硝酸为硝化试剂,使其在发烟硝酸和浓硫酸的作用下先生成硝酰氨基吡啶,再通过硝酰氨基在发烟硫酸条件下重排,最后用冰水在较低温度下萃取,制备出了高纯度高收率的2,6-二氨基-3,5-二硝基吡啶(DADNP),并对主要反应影响因素进行了研究讨论。产品经傅立叶变换红外光谱(FTIR)、氢核磁(1H-NMR)、碳核磁(13C-NMR)和高效液相色谱(HPLC)等方法进行了表征分析,结果表明是目的产物,纯度达99%以上。2,6-Diaminopyridine （DAP） was adopted as the starting material, faming nitric acid and oleum as the nitration media to prepare 2,6- diamino-3,5-dinitropyridine （DADNP） with high purity and yield. Firstly, 2, 6-dinitrylaminopyridine was synthesized in the fuming nitric acid and concentrated H2SO4 system. And then 2, 6-dinitrylaminopyridine was rearranged under the condition of oleum media. At last, 2, 6-diamino-3, 5-dinitropyridine （DADNP） was extracted from solvents by ice-water at lower temperature. The main factors which had effects on the reaction had been discussed and studied. The product was characterized by FTIR, 1H-NMR, 13C-NMR and HPLC. The result showed that the product was the aim product 2,6-diamino-3,5-dinitropyridine （DADNP）, and its purity was up to 99%.

关 键 词：2 6-二氨基-3 5-二硝基吡啶 硝化 重排 

分 类 号：TQ25[化学工程—有机化工]