2-硝基芴酮的合成

Synthesis of 2-Nitrofluorenone

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。

2-Nitrofluorenone was synthesized from fluorene by oxidation and nitration. The optimal synthetic conditions of nitration were ： H2 0 as solvent, m （fluorenone） ： m （ H2 O） = 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.