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色谱联用技术表征双格氏反应进程
引用本文:郭国建,吴立军,柳洪超,鲁毅,尤瑜生. 色谱联用技术表征双格氏反应进程[J]. 化学分析计量, 2016, 0(2): 56-59. DOI: 10.3969/j.issn.1008-6145.2016.02.016
作者姓名:郭国建  吴立军  柳洪超  鲁毅  尤瑜生
作者单位:中国兵器工业集团第五三研究所,济南,250031
摘    要:探讨双格氏试剂的结构表征方法及其制备过程跟踪分析。以1,4-二溴-2,5-对苯二甲醚为原料,在无水四氢呋喃溶剂中制备得到相应双格氏试剂,采用气相色谱–红外、气相色谱–质谱联用技术对1,4-二溴-2,5-二甲氧基苯的双格氏试剂及其反应过程中的产物进行结构表征和进程跟踪分析。结果表明,反应体系中同时存在双格氏、单格氏产物,并随着反应进行,单格氏产物进一步转化为双格氏产物。该实验结果可以对双格氏反应机理的研究提供理论数据。

关 键 词:双格氏试剂  结构表征  气相色谱联用

Characterization of Double Grignard Reaction Process by GC-MS/GC-IR
Abstract:The structure characterization of double Grignard reagent and its preparation process tracking analysis were discussed. The double Grignard reagent was prepared with 1,4-dibromo-2,5-dimethoxybenzene as raw material in the anhydrous tetrahydrofuran solvents. The structure characterization of double Grignard reagent of 1,4-dibromo-2, 5-dimethoxybenzene and its reaction process tracking analysis were carried out by GC–IR and GC–MS. The results showed that there were double grignard products and single grignard products in the reaction system at the same time,and the single product turned into the double product in the further reaction. The conclusion can providecertain theoretical data for the study of double grignard reaction mechanism.
Keywords:double Grignard reagent  structural characterization  GC combined technology
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