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对氯苯甲腈通过镍催化偶合反应合成联苯二腈研究
引用本文:佟俊,喻桂朋,刘程,蹇锡高.对氯苯甲腈通过镍催化偶合反应合成联苯二腈研究[J].辽宁化工,2008,37(2):73-76.
作者姓名:佟俊  喻桂朋  刘程  蹇锡高
作者单位:1. 大连理工大学化工学院,辽宁,大连,116012
2. 大连理工大学化工学院,辽宁,大连,116012;辽宁高性能树脂工程技术中心,辽宁,大连,116012
摘    要:对氯苯甲腈在镍催化体系中偶合生成联苯二腈的反应条件和纯化工艺进行了研究,并且对得到的联苯二甲腈的结构进行了表征.同时讨论了反应时间等对反应转化率的影响,并对粗产物提纯过程中进行了详细研究,最终得到了合成联苯二腈的工艺过程,列出最佳的反应条件.

关 键 词:对氯苯甲腈  联苯二腈  镍催化
文章编号:1004-0935(2008)02-0073-04
收稿时间:2008-01-10
修稿时间:2008年1月10日

Synthesis of 4,4'-dicyano-diphenyl by Nickel-Catalyzed Coupling of p-chlorobenzonitrile
TONG Jun,YU Gui-peng,LIU Cheng,JIAN Xi-gao.Synthesis of 4,4''''-dicyano-diphenyl by Nickel-Catalyzed Coupling of p-chlorobenzonitrile[J].Liaoning Chemical Industry,2008,37(2):73-76.
Authors:TONG Jun  YU Gui-peng  LIU Cheng  JIAN Xi-gao
Abstract:A convenient method for the synthesis of 4.4'-dicyano-dipheny together with the optimal conditions for its purification were described in this paper.4.4'-dicyano-dipheny was prepared by nickel catalyzed coupling of p-chlorobenzonitrile in the presence of excess zinc,and its structure was confirmed by Infrared ray,NMR,DSC and Elemental analysis.The influence of the reaction time and the quantity of different solvent which was used in the purification process such as distilled water and n-heptane upon the quantity of the final product also was investigated by Orthogonal experiment in detail.The yield increased exponentially with the coupling time being up to 4h.The experimental study indicated that the yield was found to be the greatest while the crude product was washed with 800 ml distilled water and 70ml n-heptane,subsequently by 30ml n-heptane three times.
Keywords:4  4'-Dicyano-dipheny  4-Chlorobenzonitrible  Nickel-Catalyzed
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