| 2-硝基芴酮的合成 |
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| 引用本文： | 张鑫,李文华,韩俊斌,吉轩,周俞君,张昭.2-硝基芴酮的合成[J].精细化工,2009,26(6). |
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| 作者姓名： | 张鑫 李文华 韩俊斌 吉轩 周俞君 张昭 |
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| 作者单位： | 山西大学,化学化工学院,山西,太原,030006 |
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| 基金项目： | 山西省教育厅高校高新技术产业化项目(20080001);;山西省研究生优秀创新项目(20081034)~~ |
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| 摘 要： | 以煤焦油分离产品芴为原料,通过氧化、硝化反应合成了2-硝基芴酮,并对硝化过程中硝酸的浓度及其用量、硫酸的用量、水的用量、反应温度和反应时间对产率的影响进行了优化选择。较佳的硝化反应条件为:水作为溶剂,m(芴酮)∶m(H2O)=1∶1.1,n(芴酮)∶n(HNO3)∶n(H2SO4)=1∶2.87∶3.60,硝酸质量分数为65%,硫酸质量分数为96%,85℃反应2 h,所得2-硝基芴酮的产率为91.7%,质量分数高于98.0%。产物结构用IR、1HNMR作了表征。
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| 关 键 词： | 芴衍生物 芴酮 2-硝基芴酮 硝化反应 精细化工中间体 |
Synthesis of 2-Nitrofluorenone |
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| ZHANG Xin,LI Wen-hua,HAN Jun-bin,JI Xuan,ZHOU Yu-jun,ZHANG Zhao.Synthesis of 2-Nitrofluorenone[J].Fine Chemicals,2009,26(6). |
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| Authors: | ZHANG Xin LI Wen-hua HAN Jun-bin JI Xuan ZHOU Yu-jun ZHANG Zhao |
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| Affiliation: | School of Chemistry and Chemical Engineering;Shanxi University;Taiyuan 030006;Shanxi;China |
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| Abstract: | 2-Nitrofluorenone was synthesized from fluorene by oxidation and nitration.The optimal synthetic conditions of nitration were:H2O as solvent,m(fluorenone)∶m(H2O)=1∶1.1,n(fluorenone)∶n(HNO3)∶n(H2SO4)=1∶2.87∶3.60,w(HNO3)=65%,w(H2SO4)=96%,reaction temperature was 80 ℃ and the reaction time was 2 h.The yield of 2-Nitrofluorenone reached 91.7% and the product purity was higher than 98.0%.The structure of product was characterized by IR and 1HNMR and 13CNMR spectra. |
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| Keywords: | fluorene derivatives fluorenone 2-nitrofluorenone nitration fine chemical intermediates |
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