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合成2,3,4-三甲氧基苯甲酸的新工艺

NEW SYNTHESIS PROCESS FOR 2,3,4-TRIMETHOXYBENZOIC ACID

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【作者】 郝永兵; 赵万胜; 董燕敏; 赵燕; 陈兴权; 赵天生;

【Author】 Hao Yongbing~(1,3),Zhao Wansheng~1,Dong Yanmin~1,Zhao Yan~1,Chen Xingquan~(1,2) and Zhao Tiansheng~2 (1.Jiangsu Key Lab of Finechemical Technology,Jiangsu Polytechnic University, Changzhou 213164,Jiangsu,China;2.Key Laboratory of Energy Resource and Chemical Engineering of Ningxia University,Yinchuan 750021,Ningxia,China;3.Department of Chemistry,Xinxing Medical University,Xinxiang 453003,He’nan,China)

【机构】 常州大学江苏精细石油化工重点实验室; 新乡医学院化学系; 宁夏大学能源化工自治区重点实验室;

【摘要】 实验以焦性没食子酸为原料,经醚化、溴代、氰化和水解等合成2,3,4-三甲氧基苯甲酸。在醚化过程中,以离子液体为催化剂,碳酸二甲酯为甲基化试剂,合成连三苯甲醚,收率为92%;连三苯甲醚经NBS溴代反应,合成2,3,4-三甲氧基溴苯,收率为92.2%;2,3,4-三甲氧基溴苯与氰化亚铜反应,合成2,3,4-三甲氧基苯腈,收率为69.5%;2,3,4-三甲氧基苯腈水解合成2,3,4-三甲氧基苯甲酸,收率为80%。

【Abstract】 2,3,4-Trimethoxybenzic acid(TMBA) was prepared from pyrogallic acid(PA) through a new route,namely etherification,bromination,cyanogenation,and then hydrolysis.PA reacted with dimethyl carbonate with an ionic liquid as catalyst.The yield of the obtained 1,2,3-trimethoxybenzene reached 92%.1,2,3-trimethoxybenzene converted to 2,3,4-trimethoxy bromobenzene with NBS.The yield of the obtained 2,3,4-trimethoxy bromobenzene was 92.2%based on 1,2,3-trimethoxybenzene. 2,3,4-trimethoxy bromobenzene reacted with cuprous cyanide in the presence of DMF as solvent.The yield of the obtained 2,3,4-trimethoxy cyanobenzene was 69.5%.TMBA was prepared by hydrolysis and acidification with the yield of 80%.The total yield of TMBA by this route was 47.2%based on PA.

【基金】 江苏省教育厅高校自然科学基础研究项目(06KJB150023)
  • 【文献出处】 精细石油化工 ,Speciality Petrochemicals , 编辑部邮箱 ,2011年01期
  • 【分类号】TQ245
  • 【被引频次】6
  • 【下载频次】361
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