| 2,7-二溴芴酮与锌汞齐和浓盐酸还原反应制备2,7-二溴芴 |
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| 引用本文： | 张鑫,韩玲翠,马广文,陈婷,张昭.2,7-二溴芴酮与锌汞齐和浓盐酸还原反应制备2,7-二溴芴[J].精细化工,2007,24(9):932-935. |
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| 作者姓名： | 张鑫 韩玲翠 马广文 陈婷 张昭 |
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| 作者单位： | 1. 山西大学,化学化工学院,山西,太原,030006
2. 太原理工大学,化学化工学院,山西,太原,030024 |
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| 摘 要： | 以2,7-二溴芴酮为原料,锌汞齐和浓盐酸为还原剂,在乙醇中还原反应制备得到了2,7-二溴芴。对反应过程中还原剂用量、溶剂、反应温度、反应时间、盐酸用量及其加入方式进行了优化选择。实验结果表明,较佳的反应条件为:以质量分数95%的乙醇为溶剂,锌汞齐和浓盐酸为还原剂,分8~10次加入浓盐酸,回流反应8 h,产率84.9%~85.4%,质量分数高于99.0%。对2,7-二溴芴酮与还原剂的摩尔比以及还原剂中的锌汞齐与盐酸的摩尔比进行了考察,其中n(2,7-二溴芴酮)∶n(锌)=1∶5,锌汞齐中n(锌)∶n(汞)=48∶1,还原剂中n(锌)∶n(HCl)=1∶6时取得了较好效果。所合成化合物的结构通过红外、核磁共振波谱进行了表征。该方法的新颖性,已为山西省科学技术情报研究所2007年3月9日提供的《检索报告》所证实。
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| 关 键 词： | 2 7-二溴芴 2 7-二溴芴酮 锌汞齐 还原 精细化工中间体 |
| 文章编号： | 1003-5214（2007）09-0932-04 |
| 修稿时间： | 2007-01-23 |
Preparation of 2,7-Dibromofluorene by Reduction of 2,7-Dibromofluorenone with Zinc Amalgam and Hydrochloric Acid |
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| ZHANG Xin,HAN Ling-cui,MA Guang-wen,CHEN Ting,ZHANG Zhao.Preparation of 2,7-Dibromofluorene by Reduction of 2,7-Dibromofluorenone with Zinc Amalgam and Hydrochloric Acid[J].Fine Chemicals,2007,24(9):932-935. |
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| Authors: | ZHANG Xin HAN Ling-cui MA Guang-wen CHEN Ting ZHANG Zhao |
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| Affiliation: | School of Chemistry and Chemical Engineering, Shanxi University, Taiyuan 030006, Shanxi, China ; School of Chemistry and Chemical Engineering, Taiyuan University of Technology, Taiyuan 030006, Shanxi, China |
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| Abstract: | 2,7-Dibromofluorene was prepared from 2,7-dibromofluorenone by reduction with zinc amalgam and hydrochloric acid in ethanol(w(C2H5OH)=95%).The optimum reaction conditions were:n(2,7-dibromofluorenone)∶n(Zn)=1∶5,n(Zn)∶n(Hg)=48∶1,n(Zn)∶n(HCl)=1∶6,adding the hydrochloric acid in 8～10 portions and refluxing for 8 h.Yield of 2,7-dibromofluorene reached 84.9%～85.4%,and purity of the product was higher than 99.0%.Structure of the product was characterized by IR and 1HNMR.The originality of this method has been proved by the search report provided by the Science and Technology Information Institution of Shanxi Province on March 9th,2007. |
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| Keywords: | 2 7-dibromofluorene 2 7-dibromofluorenone zinc amalgam reduction fine chemical intermediate |
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