| 对溴碘苯的合成研究 |
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| 引用本文： | 郭敬,白雪峰,吕宏飞.对溴碘苯的合成研究[J].化学与粘合,2009,31(6):17-18. |
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| 作者姓名： | 郭敬 白雪峰 吕宏飞 |
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| 作者单位： | 郭敬,GUO Jing(黑龙江大学,化学化工与材料学院,黑龙江,哈尔滨,150080);白雪峰,BAI Xue-Feng(黑龙江大学,化学化工与材料学院,黑龙江,哈尔滨,150080;黑龙江省科学,院石油化学研究院,黑龙江,哈尔滨,150040);吕宏飞,LV Hong-fei(黑龙江省科学,院石油化学研究院,黑龙江,哈尔滨,150040) |
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| 基金项目： | 哈尔滨市科技改关项目 |
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| 摘 要： | 以工业品对溴苯胺为原料,经重氮化、碘代合成了对溴碘苯。考察了酸介质、硫酸质量分数、有机溶剂的加入及碘代温度对收率的影响,得出较佳的合成条件：先将0.02mol对溴苯胺溶解在质量分数为20%的硫酸介质中,与0.021molNaNO2在-10℃下反应生成对溴苯基重氮硫酸盐,然后在溶液中加入氯仿与0.021molKI进行碘代反应,经简单后处理得到对溴碘苯粗产品（其中对溴碘苯HPLC纯度为98.4%）,提纯后总收率达80%,较改进前提高了15%。产物经IR和1HNMR进行了结构表征。改进后的方法大大提高了粗产品的纯度,避免了过柱子带来的麻烦,操作简便安全,过程易于控制,成本较低,更适于对溴碘苯的制备。
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| 关 键 词： | 对溴碘苯 重氮化 碘代 |
Synthesis of p-Bromoiodobenzene |
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| GUO Jing,BAI Xue-Feng,LV Hong-fei.Synthesis of p-Bromoiodobenzene[J].Chemistry and Adhesion,2009,31(6):17-18. |
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| Authors: | GUO Jing BAI Xue-Feng LV Hong-fei |
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| Affiliation: | GUO Jing, BAI Xue-Feng,LV Hong-fei ( 1.College of Chemistry and Material Science, Heilongjiang University, Harbin 150080, China;2.Institute of Petrochemistry, Heilongjiang Academy of Sciences, Harbin 150040, China) |
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| Abstract: | The p-bromoiodobenzenc was synthesized with p-bromoaniline via the sequence of diazotization and then iodine-generation. An optimized process was obtained by investigating the influence of acids,mass fraction of H2SO4,organic solvent and also iodine-generation temperature on the product yield： 0.02mol raw material dissolved into 20% sulfuric acidandthen reacted with 0.021mol NaNO2 at -10℃ followed by adding chloroform and 0.021mol KI. After simple process, the product was obtained. The purity was 98.4%（HPLC） and yield was 80% which was 15% higherthan that of unimprovement. The product was characterized by IR and ^1HNMR.The purity of crude matter was enhanced by the facile method, avoiding the trouble from chromatogram method. This method was fit for synthesis of p-bromoiodobenzene. |
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| Keywords: | p-Bromoiodobenzene diazotization iodine-generation |
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