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间接电还原制备4-氯-3,5-二氨基苯甲腈
引用本文:高乾善,颜国刚,吕瑞敏,高光杰,胡建强.间接电还原制备4-氯-3,5-二氨基苯甲腈[J].山东化工,2009,38(2):4-7.
作者姓名:高乾善  颜国刚  吕瑞敏  高光杰  胡建强
作者单位:1. 山东省分析测试中心,山东,济南,250014
2. 山东博士伦福瑞达制药有限公司,山东,济南,250101
摘    要:采用间接电化学还原路线,在离子膜电解槽中,以铜板作阴极电极,石墨作阳极电极,电流密度50mA/cm^2,将Sn^4+还原为Sn^2+,然后用该电解液还原4-氯-3,5-二硝基苯甲腈为4-氯-3,5-二氨基苯甲腈。实验结果表明,盐酸浓度为4mol/mL。反应温度20℃,Sn^2+与4-氯-3,5-二硝基苯甲腈的物质的量之比为6.6/1有最佳的反应效果。母液循环试验5次,平均产率88.1%。平均电解效率74.2%。

关 键 词:4-氯-3  5-二硝基苯甲腈  4-氯-3  5-二氨基苯甲腈  间接电还原  制备

Preparation of 4-Chloro-3,5-diaminobenzonitrile by Indirect Electroreduction Method
GAO Qian-shan,YAN Guo-gang,LU Rui-min,GAO Guang-jie,HU Jian-qiang.Preparation of 4-Chloro-3,5-diaminobenzonitrile by Indirect Electroreduction Method[J].Shandong Chemical Industry,2009,38(2):4-7.
Authors:GAO Qian-shan  YAN Guo-gang  LU Rui-min  GAO Guang-jie  HU Jian-qiang
Affiliation:1.Shandong analysis And Test Center;Jinan 250014;China;2.Shandong Bausch & Lomb Freda Pharmaceutical.Co.;Ltd.;Jinan 250101;China
Abstract:4 -Chloro- 3,5 -diaminobenzonitrile was prepared by indirect electrochemistry reduction. At first, Sn^4+ was reduced to Sn^2+ in ionic membrane electrolytic cell using the copper plate as negative electrode and the graphite as anode electrode, and the current density was 50mA/cm^2, then, 4 - ehloro - 3,5 - dinitrobenzonitrile was reduced to the product by the electrolyte. The optimum react conditions were given in this paper. The concentration of HCl was 4.0 mol/L, and the react temperature was 20℃, and the molar ratio of Sn^2+ and 4 - chloro - 3,5 - dinitrobenzonitrile was 6.6/1. The recycle use of the mediator was also studied and the average yield of product was 88.1%. and the average current efficiency was 74.2%.
Keywords:4-chloro-3  5-dinitrobenzonitrile  5-diaminobenzonitrile  indirect electroreduction  preparation    
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