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5-硝基愈创木酚钠的合成

THE SYNTHESIS OF SODIUM 5-NITROGUAIACOLATE

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【作者】 古凤才王金明范国梁钟卫民

【Author】 GU Feng cai 1, WANG Jin ming 1, FAN Guo liang 2, ZHONG Wei min 1 (1. Department of Chemistry, Tianjin University, 300072 China; 2. Analysis Center, Tianjin University, 300072 China)

【机构】 天津大学化学系!天津300072天津大学分析中心!天津300072

【摘要】 报道了5-硝基愈创木酚钠(5-NGS)的合成方法。由愈创木酚与乙酐在100℃回流1 h 得到乙酰化产物。反应中生成的乙酸不必分离,再补加一定量乙酸作为下一步反应的溶剂。用发烟硝酸直接硝化上述乙酰化物,总收率高于70% 。用IR、1HNMR和MS对产物的结构进行了表征

【Abstract】 The synthesis of sodium 5 nitroguaiacolate (5 NGS) was studied by direct nitration of guaiacol acetate. Firstly, the guaiacol was acetylated by refluxing it with acetic anhydride and trace concentrated sulfuric acid as catalyst at 100℃ for 1 h. The acetic acid formed in the reaction needed not to remove and the stoichiometrical acetic acid which is as solvent for next reaction was added. The solution of guaiacol acetate in glacial acetic acid was nitrated by fuming nitric acid directly under 10℃. The total yield of 5 NGS obtained from experiments was above 70%. The structure of 5 NGS were also studied by IR, 1HNMR, and MS.

  • 【文献出处】 化学反应工程与工艺 ,CHEMICAL REACTION ENGINEERING AND TECHNOLOGY , 编辑部邮箱 ,1999年04期
  • 【分类号】TQ452
  • 【被引频次】9
  • 【下载频次】189
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