第 39 卷第 6 期Vol. 39 No. 6
2009 年 12 月Dec 2009

所属栏目:医药及中间体

Kyodai硝化法合成1-硝基金刚烷
张 琳,马 伟,罗 军 (南京理工大学 化工学院,江苏 南京 210094)
摘 要:将二氧化氮-臭氧体系用于金刚烷的直接硝化合成重要中间体1-硝基金刚烷,研究二氧化氮用量、反应时间、反应温度和臭氧流量等因素对反应的影响,在n(金刚烷) ∶ n(二氧化氮)=1 ∶ 15、臭氧流量为0.4 L/min、-30℃下反应2 h的优化条件下,金刚烷的转化率为99.9%,1-硝基金刚烷的收率为90.9%,当n(金刚烷) ∶ n(二氧化氮)=1 ∶ 30时,1-硝基金刚烷的收率可达92.1%。
关键词:1-硝基金刚烷;金刚烷;Kyodai硝化;绿色化学工艺
中图分类号:O623.71  文献标识码:A  文章编号:1009-9212(2009)06- 0022-03
Synthesis of 1-Nitroadamantane via Kyodai Nitration
ZHANG Lin,MA Wei,LUO Jun (School of Chemical Engineering,Nanjing University of Science and Technology,Nanjing 21009,China)
Abstract:1-Nitroadamantane was synthesized from adamantine by direct nitration with NO2-O3. The reaction afforded 1-nitroadamantane in 90.9% yield with adamantine conversion of 99.9% under the optimized conditions:n(adamantine)∶ n(NO2)= 1 ∶ 15,flow rate of O3 = 0.4 L/min,reaction temperature -30℃,reaction time 2 h. Moreover,when 30 equivalents of NO2 was used,1-nitroadamtane was obtained in a higher yield of 92.1%. This technology avoids use of nitrous acid,and therefore is a green process.
Key words:1-nitroadamantane;adamantine;Kyodai nitration;green chemical process
作者简介:张 琳(1976 ),女,河南南阳人,讲师,博士,主要从事含能材料研究。(E-mail:l_njust@yahoo.com.cn)
收稿日期:2009-11-16