2,2'-二氨基联苄的合成研究  

Study on the synthesis of 2,2′-diaminodibenzyl

作　　者：宋国强[1] 唐龙[1] 王羚竹[1] 王瑞瑞[1] 冯筱晴[1,2] 

机构地区：[1]常州大学制药与生命科学学院,江苏常州213164 [2]常州市药品制造与质量控制工程重点实验室,江苏常州213164

出　　处：《应用化工》2013年第3期436-439,共4页Applied Chemical Industry

基　　金：江苏省研究生科研创新计划项目(CXZZ12_0730)

摘　　要：以邻硝基氯苄为起始原料,经缩合和还原得到2,2'-二氨基联苄,探索了反应的影响因素。结果表明,2,2'-二硝基联苄较佳合成条件为:n(邻硝基氯苄)∶n(金属钠)=1∶2,回流,反应7 h,收率85.00%,HPLC纯度97.32%;2,2'-二氨基联苄的较佳合成条件:n(2,2'-二硝基联苄)∶n(Fe)=1∶7,采用水与无水乙醇混合溶剂,V(水)∶V(乙醇)=2∶1,反应时间4 h,反应温度90℃,收率97.50%,HPLC纯度98.86%。产品结构经1H NMR、13C NMR和LC-MS分析表征确认。Abstraet：o-Nitrobenzyl chloride was reduced to prepare 2,2＇-diaminodibenzyl. The experimental condi- tions,such as materials ratio, reaction temperature and reaction time were investigated. Results showed that the optimal condition for condensation reaction were found as：n （o-nitrobenzyl chloride） ： n （Na） = 1 ：2,reflux time 7 h,under which the yield of 2,2＇-dinitrodibenzyl was 85% based on o-nitrobenzyl chlo- ride and the purity was 97.32% as determined by HPLC ; proper reduction reaction conditions were found as ： n （2,2＇-dinitrodibenzyl） ： n （Fe） = 1 ： 7, H20 and C2 H5 OH as solvent, V（ H2 O） ： V（ C2 H5 OH） = 2 ： 1, reaction temperature 90℃, reaction time 4 h, under which the yield of 2,2＇-diaminodibenzyl was 97.5 % based on 2,2＇-dinitrodibenzyl and the purity was 98.86% as determined by HPLC. The molecular structures of product were identified by ^1H NMR, ^13C NMR and LC-MS. Key words ：2,2＇-diaminodibenzyl; synthesis ; o-nitrobenzyl chloride ; 2,2＇-dinitrodibenzyl

关 键 词：2 2'-二氨基联苄 合成 邻硝基氯苄 2 2'-二硝基联苄 

分 类 号：TQ246.3[化学工程—有机化工]