| 2-羟基-4,6-二甲氧基脱氧安息香催化合成工艺 |
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| 引用本文： | 吴纯鑫,吴秋萍,李阳阳,赵德明,陈英奇. 2-羟基-4,6-二甲氧基脱氧安息香催化合成工艺[J]. 化工进展, 2011, 30(5): 1089-1092 |
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| 作者姓名： | 吴纯鑫 吴秋萍 李阳阳 赵德明 陈英奇 |
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| 作者单位： | 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 |
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| 基金项目： | 浙江省教育厅基金，浙江省高校青年教师资助计划项目 |
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| 摘 要： | 以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AlCl3与1,3,5-三甲氧基苯的摩尔配比1.1∶1，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1.2∶1，反应温度82 ℃。产品经1H NMR、MS进行了结构表征。
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| 关 键 词： | 2-羟基-4,6-二甲氧基脱氧安息香 2,4,6-三甲氧基脱氧安息香 Houben-Hoesch反应 Friedel-Crafts反应 |
Catalytic synthesis process of 2-hydroxy-4,6-dimethoxydeoxybenzoin |
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| WU Chunxin,WU Qiuping,LI Yangyang,ZHAO Deming,CHEN Yingqi. Catalytic synthesis process of 2-hydroxy-4,6-dimethoxydeoxybenzoin[J]. Chemical Industry and Engineering Progress, 2011, 30(5): 1089-1092 |
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| Authors: | WU Chunxin WU Qiuping LI Yangyang ZHAO Deming CHEN Yingqi |
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| Affiliation: | 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 |
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| Abstract: | 2-Hydroxy-4,6-dimethoxydeoxybenzoin was synthesized from 1,3,5- trimethoxybenzene，via the Houben-Hoesch reaction or Friedel-Crafts reaction and demethylation of 2,4,6- trimethoxydeoxybenzoin. Because of the protection of methyl group，the 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 investigated，and the optimal process parameters were as follows：（1）in Friedel-Crafts reaction，the ratio of catalyst（aluminum chloride）and 1,3,5-trimethoxybenzene 1.1∶1，reaction temperature 25 ℃，（2）in demethylation，the ratio of demethylation reagent and 2,4,6- trimethoxydeoxybenzoin 1.2∶1，reaction temperature 82 ℃. The product was characterized with 1H NMR and MS. |
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