化工进展

• 精细化工 • 上一篇    下一篇

2-羟基-4,6-二甲氧基脱氧安息香催化合成工艺

吴纯鑫1,吴秋萍1,李阳阳1,赵德明1,陈英奇2   

  1. 1浙江工业大学化学工程与材料材学院,浙江 杭州310014;2浙江大学材料与化学工程学院,浙江 杭州 310027
  • 出版日期:2011-05-05 发布日期:2011-05-05

Catalytic synthesis process of 2-hydroxy-4,6-dimethoxydeoxybenzoin

WU Chunxin1,WU Qiuping1,LI Yangyang1,ZHAO Deming1,CHEN Yingqi2   

  1. 1College of Chemical Engineering and Materials Science,Zhejiang University of Technology,Hangzhou 310014,Zhejiang,China;2 College of Material and Chemical Engineering,Zhejiang University,Hangzhou 310027,Zhejiang,China
  • Online:2011-05-05 Published:2011-05-05

摘要:

1,3,5-三甲氧基苯为原料,经Houben-Hoesch反应或Friedel-Crafts酰化反应得到2,4,6-三甲氧基脱氧安息香后选择性脱去2位甲基,得到2-羟基-4,6-二甲氧基脱氧安息香目标产品。因甲基的保护作用降低了羟基的反应活性,使Houben-Hoesch反应单步收率提高到81.3%Friedel-Crafts酰化反应收率达94.5%,脱甲基反应收率达93.8%。考察了催化剂用量、温度等因素的影响,优化选择了各反应的较佳工艺参数。Friedel-Crafts酰基化反应中,催化剂AlCl31,3,5-三甲氧基苯的摩尔配比1.11,反应温度25 (室温);脱甲基反应中,脱甲基试剂与2,4,6-三甲氧基脱氧安息香的摩尔配比1.21,反应温度82 。产品经1H NMRMS进行了结构表征。

Abstract:

2-Hydroxy-4,6-dimethoxydeoxybenzoin was synthesized from 1,3,5- trimethoxybenzenevia the Houben-Hoesch reaction or Friedel-Crafts reaction and demethylation of 2,4,6- trimethoxydeoxybenzoin. Because of the protection of methyl groupthe reactivity of hydroxy groups was reduced and the yields of Houben-Hoesch and Friedel-Crafts reaction reached to 81.3% and 94.5% respectively. The yield of demethylation was 93.8%. The effects of catalyst amount and reaction temperature were investigatedand the optimal process parameters were as follows:(1in Friedel-Crafts reactionthe ratio of catalystaluminum chlorideand 1,3,5-trimethoxybenzene 1.11reaction temperature 25 ,(2in demethylationthe ratio of demethylation reagent and 2,4,6- trimethoxydeoxybenzoin 1.21reaction temperature 82 . The product was characterized with 1H NMR and MS.

京ICP备12046843号-2;京公网安备 11010102001994号
版权所有 © 《化工进展》编辑部
地址:北京市东城区青年湖南街13号 邮编:100011
电子信箱:hgjz@cip.com.cn
本系统由北京玛格泰克科技发展有限公司设计开发 技术支持:support@magtech.com.cn