5-溴苊的合成研究

Study on the Synthesis of 5-Bromoacenaphthene

以苊为原料,采用两种氧化溴化体系合成5-溴苊,确定较佳的溴化体系及溴化工艺条件。考察了溶剂种类、物料配比、反应温度及时间对反应收率的影响。实验结果表明:在乙酸乙酯溶剂中,反应温度20℃,反应时间为1h,n(溴酸钠)∶n(亚硫酸氢钠)∶n(苊)=1.2∶1.2∶1,产品收率为85.8%,纯度﹥98%(HPLC)。产品结构经IR和1 H NMR表征。

5-Bromoacenaphthene was synthesized from acenaphthene via two different oxybromination system. The better oxybromination system and brominated process conditions were determined. The optimal reaction conditions, such as the different solvent, the raw material ratio, reaction temperature and reaction time were found. The experimental results showed that the yield of product was 85.8% and the purity was greater than 98%（HPLC） ,when the reaction was carried out for lh at 20℃ using ethyl acetate as soluent and the ratio of reagent was n（sodium bromate） ： n（sodium bisulfite） ： n（acenaphthene） = 1.2 ; 1.2 ： 1. The chemical structure of the product was characterizde by IR and H NMR.