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机构地区:[1]天津大学化学系,天津300072 [2]天津大学分析中心,天津300072
出 处:《化学反应工程与工艺》1999年第4期454-456,共3页Chemical Reaction Engineering and Technology
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。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.
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