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以对硝基苯乙酮为原料、氯化亚锡为还原剂,制备了对氨基苯乙酮,产率为68.0%.在0~5℃下对对氨基苯乙酮进行氯化和溴化,制备了3,5-二氯对氨基苯乙酮和3,5-二溴对氨基苯乙酮,产率分别为52.7%、60.8%.在亚硝酸钠盐酸体系下对中间体进行重氮化,以次磷酸为质子化试剂,合成了目标产物3,5-二氯苯乙酮和3,5-二溴苯乙酮,产率分别为60.2%、63.3%.并用FTIR、MS对其结构进行了表征.
Abstract:P-aminoacetophenone was prepared from p-nitroacetophenone using SnCl2 as the reducing agent.The yield rate was 68.0 %.3,5-dichloro-p-aminoacetophenone and 3,5-dibromo-p- aminoacetophenone were prepared from p- aminoacetophenone by chhorination and bromination at 0~5℃.The yield rates were 52.7 % and 60.8 % respectively. After diazotization in the sodium nitrite-hydrochloric acid system and protonation by hypophosphorous acid,the aim compounds were yielded 60.2 % and 63.3 % respectively.All the compounds were characterized by FTIR and MS.
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基本信息:
DOI:
中图分类号:TQ244.4
引用信息:
[1]汤艳峰,朱金丽,孙同明等.3,5-二氯(溴)苯乙酮的合成与表征[J].南通大学学报(自然科学版),2008,7(04):53-55.
基金信息:
南通大学自然科学基金项目(06Z017);; 南通市科技局项目(K2007011)