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机构地区:[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
出 处:《化工中间体》2009年第3期30-33,共4页
摘 要:利用瑞乃镍作催化剂,丙酮作溶剂,在加氢控制剂作用下将4-氯-3,5-二硝基苯甲腈(CDNBN)选择性氢化还原,得到4-氯-3,5-二氨基苯甲腈(CDABN)。文中探讨了温度、氢气压力、控制剂、催化剂等对反应的影响。确定了最佳生产工艺条件:反应温度40℃,氢气压力2.0-3.0MPa,CDNBN:控制剂:催化剂为40:1.0:4.0。实验结果证明,CDNBN平均转化率为98.7%,CDABN平均产率93.4%,重结晶后的平均产率为90.5%。using Raney Nickel as catalyst, acetone as solvent, by the action of hydrogenation control agent, the 4-chloro-3,5-diaminobenzonitrile (CDABN) was prepared by selective hydrogenation reduction from 4-chloro-3,5-dinitrobenzonitrile (CDNBN). The effects on the reaction such as temperature pressure and control agent and catalyst were discussed. The optimum reaction conditions were confirmed as follows: the reaction temperature was 40℃, the pressure of hydrogen was 2.0-3.0MPa, the weight ratio of CDNBN:control agent:catalyst was 40:1.0:4.0. The results proved that the average ratio conversion of CDNBN is 98.7%and the average yield of CDABN is 93.4%(by HPLC), the average yield by recrystallization is 90.5%.
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