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联苯类化合物4′-氯-2-硝基联苯的绿色合成新工艺与晶体结构
NewGreen Synthetic Process and Crystal Structrue of 4′-Chloro-2-Nitrobiphenyl
【摘要】 对4′-氯-2-硝基联苯的合成路线进行优化,以获得适合工业化生产的工艺路线。以对氯溴苯和邻溴硝基苯为原料,以Pd(dppf)Cl~2为催化剂,依次经过格氏反应、Suzuki偶联两步反应合成4′-氯-2-硝基联苯。X-射线衍射测定了其晶体结构。在优化的反应条件下,4′-氯-2-硝基联苯的合成总收率≥82%,纯度98.8%;产物结构经IR、~1H NMR、MS确证。该工艺绿色环保,条件温和,适合工业化生产。
【Abstract】 To develop a new synthetic route of 4′-chloro-2-nitrobiphenyl by optimizing the reported synthesis routes and the product was characterized.4′-Chloro-2-nitrobiphenyl was prepared using 4-bromochlorobenzene and 1-bromo-2-nitrobenzene as starting material by a series of Grignard reaction and Suzuki coupling reaction.Under the optimal reaction conditions, the total yield of 4′-Chloro-2-Nitrobiphenyl was over 82% based on 4-bromochlorobenzene, the purity was 98.8%.The structure was confirmed by IR,~1H NMR,MS.This process is green, warm and economical, which is suitable for industrial scale manufacture
【Key words】 4′-chloro-2-nitrobiphenylor; new synthetic process; crystal structure;
- 【文献出处】 应用化工 ,Applied Chemical Industry , 编辑部邮箱 ,2019年S1期
- 【分类号】TQ455.4
- 【下载频次】38