水解萃取法合成愈创木酚的工艺路径  

Synthesis Process of Guaiacol Combining the Technology of Hydrolysis-Extraction

作　　者：申屠有德 舒卫进 姚跃良 毛海舫 SHENTU Youde;SHU Weijin;YAO Yueliang;MAO Haifang(Shandong Apeloa Hanxing Pharmaceutical Co.,Ltd.,Changyi 261312,Shandong,China;Zhejiang Apeloa Jiayuan Pharmaceutical Co.,Ltd.,Dongyang 322118,Zhejiang,China;Shanghai Institute of Technology,Shanghai 201418,China)

机构地区：[1]山东普洛汉兴医药有限公司,山东昌邑261312 [2]浙江普洛家园药业有限公司,浙江东阳322118 [3]上海应用技术大学,上海201418

出　　处：《香料香精化妆品》2022年第6期1-4,共4页Flavour Fragrance Cosmetics

摘　　要：采用邻氨基苯甲醚为原料,经重氮化反应得重氮盐溶液,再以硫酸铜为催化剂,甲苯为萃取剂,用水解萃取耦合新技术制备愈创木酚。讨论了搅拌速度、重氮盐溶液含量、硫酸铜的起始含量以及甲苯用量等对反应的影响。结果表明,在质量分数为7%的重氮液、质量分数为50%的硫酸铜、甲苯与水相体积比为1:1、水解温度为81~82℃时可以保证水解反应的顺利进行,达到最佳萃取效果和分层溢流的目的,反应收率可达90.80%,纯化后产品纯度达99.74%。该方法具有降低水解反应温度,提高反应选择性,降低生产能耗及成本,易于工业化生产等优点。A novel process for the synthesis of guaiacol combining the hydrolysis-extration technology was developed,starting from O-anisidine, via diazotization reaction and CuSO4-catalyzed hydrolyzation reaction, meanwhile using toluene as the extracting agent. Effects of stirring speed, concentrations of diazonium salt solution and CuSO4, dosage of toluene on the hydrolyzation reaction were discussed. The results showed that the optimal reaction conditions(yield up to 90.80%and purity up to 99.74%) were 7%(mass fraction) of the diazonium salt solution, 50%(mass fraction) of CuSO4 solution,1:1 of the volume ratio for toluene and aqueous phase at 81-82℃. The method has many advantages, such as lowering the temperature of the hydrolyzation reaction, improving the reaction selectivity, reducing the energy consumption and cost, easy to industrialization and so on.

关 键 词：催化 水解萃取 重氮化 邻氨基苯甲醚 愈创木酚 

分 类 号：TQ243.12[化学工程—有机化工]