3,3,5,5-四甲基联苯胺的合成研究
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摘要
3,3,5,5-四甲基联苯胺是一种重要的色原试剂。本文以2,6-二甲基苯胺为原料,经过活化、氧化偶联和提纯,得到纯品3,3,5,5-四甲基联苯胺,总收率达到65%。产品经过核磁氢谱和核磁碳谱表征。该路线能有效减少副产物。
The important chromogen reagent,3,3 5,5-Tetramethylbenzidine,was synthesized by the reaction of excitation,oxidation coupled and purification,using 2,6-dimethylaniline as the starting material. An overall yield of 65% was achieved. The structure was confirmed by ~1H NMR and ~(13)C NMR. This method can reduce by-product effectively.
The important chromogen reagent,3,3 5,5-Tetramethylbenzidine,was synthesized by the reaction of excitation,oxidation coupled and purification,using 2,6-dimethylaniline as the starting material. An overall yield of 65% was achieved. The structure was confirmed by ~1H NMR and ~(13)C NMR. This method can reduce by-product effectively.
引文
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[4]朱雯芳,乔江彬,卓广澜.钯碳催化下以甲酰肼为还原剂的卤代芳烃还原偶联反应研究[J].有机化学,2008,28(7):1259-1263.
[5]方智慧,刘贤奎.TMB反应产物稳定方法的改进[J].河南医科大学学报,1992,27(4):365-366.
[6]施士雄,徐正璋.ELISA新底物TMB终止剂的研究[J].上海免疫学杂志,1991,11(4):222-224.
[7]Hare S,Smith S J,Metifiot M,et al.Structural and functional analyses of the second-generation integrase strand transfer inhibitor dolutegravir (S/GSK 1349572)[J].Mol Pharmacol,2011,80(4):565-572.
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[9]吴生文,田重威,胡四明,等.一种光学活性的3-氨基丁醇和3-氨基丁醇的制备方法:CN,104370755 A[P].2015-02-25.
[10]丁军委,孙国庆,刘宝,等.2,2-二氯氢化偶氮苯重排生成3,3-二氯联苯胺的研究[J].精细石油化工进展,2008,4(9):31-33.
[11]刘旭锋,钟增培,许京丽,等.三芳基咪唑类化合物的合成及其双光子吸收性能研究[J].分析测试学报,2006,25(3):6-10.
[12]叶菲,赵李霞,付颖.手性化合物S-(+)-和R-(-)-2-氨基丁醇的制备方法:CN,101863779 A[P].2010-10-20.
[2]廖联安,郭奇珍.3,3,5,5-四甲基联苯胺的合成[J].中国医药工业杂志,1998,27(3):126-127.
[3]于宏伟,段书德,刘会茹,等.2,6-二烷基-4-溴苯胺的合成及表征[J].化学试剂,2009,31(9):757-758.
[4]朱雯芳,乔江彬,卓广澜.钯碳催化下以甲酰肼为还原剂的卤代芳烃还原偶联反应研究[J].有机化学,2008,28(7):1259-1263.
[5]方智慧,刘贤奎.TMB反应产物稳定方法的改进[J].河南医科大学学报,1992,27(4):365-366.
[6]施士雄,徐正璋.ELISA新底物TMB终止剂的研究[J].上海免疫学杂志,1991,11(4):222-224.
[7]Hare S,Smith S J,Metifiot M,et al.Structural and functional analyses of the second-generation integrase strand transfer inhibitor dolutegravir (S/GSK 1349572)[J].Mol Pharmacol,2011,80(4):565-572.
[8]Cooper D A,Steigbigel R T,Gatell J M,et al.Subgroup and resistance analyses of raltegravir for resistant HIV-1 infection[J].N Engl J Med,2008,359(4):355-365.
[9]吴生文,田重威,胡四明,等.一种光学活性的3-氨基丁醇和3-氨基丁醇的制备方法:CN,104370755 A[P].2015-02-25.
[10]丁军委,孙国庆,刘宝,等.2,2-二氯氢化偶氮苯重排生成3,3-二氯联苯胺的研究[J].精细石油化工进展,2008,4(9):31-33.
[11]刘旭锋,钟增培,许京丽,等.三芳基咪唑类化合物的合成及其双光子吸收性能研究[J].分析测试学报,2006,25(3):6-10.
[12]叶菲,赵李霞,付颖.手性化合物S-(+)-和R-(-)-2-氨基丁醇的制备方法:CN,101863779 A[P].2010-10-20.