第 45 卷第 5 期 Vol. 45 No. 5 2015 年 10 月 Oct 2015

所属栏目：功能材料 一锅法合成3-硝基吡唑的研究

刘 威1，2，李永祥2*，许元刚1，2，刘 伟2 （1. 南京理工大学 化工学院，江苏 南京 210094；2.中北大学 化工与环境学院，山西 太原 030051）

摘　要：以吡唑为原料，经发烟硝酸和醋酐体系硝化后，将反应液在水热釜中高压反应，一锅法合成了3-硝基吡唑。产物经红外光谱、熔点、高效液相色谱表征。优化反应条件为：4.0 g吡唑、4.4 mL发烟硝酸、10.7 mL醋酐在冰水浴中反应1 h，然后将得到的反应液在170℃下、在水热釜中高压密封反应3 h，3-硝基吡唑的收率达46.2%。

关键词：一锅法；3-硝基吡唑；高压反应

中图分类号：TJ55　　文献标识码：S　　文章编号：1009-9212（2015）05-0060-03

One-pot Method for Synthesis of 3-Nitropyrazole

LIU Wei1,2, LI Yong-xiang2*, XU Yuan-gang1,2, LIU Wei2 (1. School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China; 2. School of Chemical and Environmental Engineering, North University of China, Taiyuan 030051, China)

Abstract：3-Nitropyrazole was synthesized using pyrazole as the starting material by one-pot method. In this method, pyrazole was nitrated using fuming nitric acid and acetic anhydride; Then, the obtained liquid was transferred to a hydrothermal reaction vessel and reacted under a condition of high-pressure. The target product was characterized by IR, melting point and HPLC. A typical process under the optimal reaction condition was as following: pyrazole(4.0 g) in the mixture of fuming nitric acid(4.4 mL) and acetic anhydride(10.7 mL) was nitrated for 1 h at a temperature which was controlled by an ice-water bath; then, the obtained liquid was reacted under high-pressure for 3 h at 170℃ in a hydrothermal reaction vessel. The yield rate was 46.2%.

Key words：one-pot; 3-nitropyrazole; high-pressure reaction

作者简介：刘 威（1992-），男，湖北孝感人，硕士研究生，主要从事炸药合成研究（E-mail：1104054142@st.nuc.edu.cn）。

联 系 人：李永祥，教授，主要从事含能材料的合成及应用研究。

收稿日期： 2015-08-1