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0.4L/min、-30℃下反应2h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%。
1-Nitroadamantane was synthesized from adamantine by direct nitration with NO2-O3. The reacuon 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 03 = 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.
出处
《精细化工中间体》
CAS
2009年第6期22-24,39,共4页
Fine Chemical Intermediates
