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作 者:乔鹏伟[1] 王晓萌[1] 张鑫[1] 吉轩[1] 张鹏[1] 张昭[1]
出 处:《当代化工》2010年第6期634-636,共3页Contemporary Chemical Industry
基 金:山西省留学归国基金,项目号:200817;山西省高等学校科技项目,项目号:20080001.
摘 要:以芴为原料,通过氧化、硝化反应制备得到2,7-二硝基芴酮,并对硝化反应条件进行了优化选择。最佳的合成条件为:水作为溶剂,质量分数为65%的硝酸和质量分数为96%的硫酸混合酸为硝化试剂,分2批加入混合酸,第1次加入混合酸总用量的1/4,回流反应1 h后,继续滴加剩余的混合酸,回流反应6 h。其中n(芴酮)/n(HNO3)/n(H2SO4)=1︰10︰13,m(芴酮)/m(H2O)=1︰1.1,所得2,7-二硝基芴酮的产率为90%,质量分数〉98%。产品结构经红外、核磁共振波谱的确证。2,7-Dinitro-9-fluorenone was prepared from fluorene by oxidation and nitration.The optimal nitration conditions of 2,7-dinitro-9-fluorenone were as follows: using H2O as solvent,HNO3(65%)-H2SO4(96%) as nitrating reagent,the nitrating reagent was added dropwise at reflux by two times(amount of first addition was 1/4 of the total addition,and reaction time after each addition was 1 h and 6 h,respectively),n(fluorenone)/n(HNO3)/n(H2SO4) =1︰10︰13,m(fluorenone)/m(H2O)=1︰1.1;the yield reached 90.0% and the mass percentage was higher than 98.0%.The structures of all products were characterized by IR and NMR spectra.
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