一种2,6-二甲基苯甲酸的改进合成方法
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摘要
以2,6-二甲基苯胺为原料,通过重氮化反应制备2,6-二甲基苯腈,经水蒸汽蒸馏法提纯后,采用75%硫酸酸化,再经酸碱法对产物进行脱色和纯化得产物2,6-二甲基苯甲酸,总收率68.4%。工艺简单、操作安全、适合工业化生产。
2,6-Dimethyl benzonitrile was synthesized by diazo reaction using 2,6-dimethyl aniline as starting material. The crude 2,6-dimethyl benzonitrile was further purified by steam distillation. The purified 2,6-dimethyl benzonitrile was acidized using 75% sulfuric acid, and the obtained crude 2,6-dimethyl benzoic acid was then decolorized and purified by acid-base method to give the target product. This simple and safe procedure is suitable for production in large scale.
2,6-Dimethyl benzonitrile was synthesized by diazo reaction using 2,6-dimethyl aniline as starting material. The crude 2,6-dimethyl benzonitrile was further purified by steam distillation. The purified 2,6-dimethyl benzonitrile was acidized using 75% sulfuric acid, and the obtained crude 2,6-dimethyl benzoic acid was then decolorized and purified by acid-base method to give the target product. This simple and safe procedure is suitable for production in large scale.
引文
[1]David L S,Justin S,Steven V O,et al.Synthesis and evaluation of novel 1-(2-acylhydrazinocarbonyl)-cycloalkyl carboxamides as interleukin-1b converting enzyme(ICE)inhibitors[J].Bioorganic&Medicinal Chemistry Letters,2006,16:4 233-4 236.
[2]Ramesh G,Nathan M,Jiao-jie L,et al.Palladium-catalyzed methylation and arylation of sp2 and sp3 C-H bonds in simple carboxylic acids[J].J Am Chem Soc,2007,129:3 511.
[3]Zheng S,Yu C,Shen Z W.Ethyl cyanoacetate:a new cyanating agent for the palladium-catalyzed cyanation of aryl Halides[J].Organic Letters,2012,14:3 644-3 647.
[4]Hirai N,Tatsukawa Y,Kameda M,e t al.Aerobic oxidation of trimethylbenzenes catalyzed by N,N,N″-trihyd roxyisocyanuric acid(THICA)as a key catalyst[J].Tetrahedron,2006,62:6 695-6 699.
[5]赵迎春,张学楷,黄龙江,等.2,6-二甲基苯甲酸的合成工艺研究[J].科学技术与工程,2013,13(2):4 724-4 725.
[2]Ramesh G,Nathan M,Jiao-jie L,et al.Palladium-catalyzed methylation and arylation of sp2 and sp3 C-H bonds in simple carboxylic acids[J].J Am Chem Soc,2007,129:3 511.
[3]Zheng S,Yu C,Shen Z W.Ethyl cyanoacetate:a new cyanating agent for the palladium-catalyzed cyanation of aryl Halides[J].Organic Letters,2012,14:3 644-3 647.
[4]Hirai N,Tatsukawa Y,Kameda M,e t al.Aerobic oxidation of trimethylbenzenes catalyzed by N,N,N″-trihyd roxyisocyanuric acid(THICA)as a key catalyst[J].Tetrahedron,2006,62:6 695-6 699.
[5]赵迎春,张学楷,黄龙江,等.2,6-二甲基苯甲酸的合成工艺研究[J].科学技术与工程,2013,13(2):4 724-4 725.