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2-羟基-4-甲氧基-5-磺酸基二苯甲酮的合成

赵德明1,韩太平1,赵秋霞2,张建庭1,金宁人1   

  1. 1浙江工业大学化学工程与材料学院,浙江 杭州 310032;2杭州民生药业有限公司,浙江 杭州 310011
  • 出版日期:2011-04-05 发布日期:2011-04-05

Synthesis of 2-hydroxy-4-methoxy-5-sulfonic acid benzophenone

ZHAO Deming1,HAN Taiping1,ZHAO Qiuxia2,ZHANG Jianting1,JIN Ningren1   

  1. 1School of Chemical Engineering and Materials Sciences,Zhejiang University of Technology,Hangzhou 310032,Zhejiang,China;2Hangzhou Minsheng Pharmaceutical Group Co.,Ltd.,Hangzhou 310011,Zhejiang,China
  • Online:2011-04-05 Published:2011-04-05

摘要:

采用间苯二甲醚为原料,经酰化、脱甲基、磺化一系列的反应合成2-羟基-4-甲氧基-5-磺酸基二苯甲酮,并对其物料配比、催化剂用量、反应温度以及反应时间等因素作了探索。结果表明酰化反应较佳条件为:以二氯甲烷为溶剂,n(间苯二甲醚)n(苯甲酰氯)n(无水AlCl3)=11.051.05,反应温度05 ,反应时间3 h。脱甲基反应较佳条件为:以二氯甲烷为溶剂,n(2,4-二甲氧基二苯甲酮)n(无水AlCl3)=11.051.10,反应温度2025 ,反应时间3 h;磺化反应较佳条件为:以乙酸乙酯为溶剂,n(2-羟基-4-甲氧基二苯甲酮)n(氯磺酸)=11.05,室温反应12 h。以间苯二甲醚计总收率为72.35%2-羟基-4-甲氧基-5-磺酸基二苯甲酮的HPLC度为99.31%2-羟基-4-甲氧基-5-磺酸基二苯甲酮及中间体产品结构经1H-NMR13C-NMR FT-IR分析表征确认。

Abstract:

Through acetylationdemethylation and sulfonation2-hydroxy-4- methoxy-5-sulfonic acid benzophenone was synthesized from resorcinol and the experimental conditionssuch as materials ratioreaction temperature and reaction timewere investigated. Proper experimental conditions for acetylation reaction were found asn1,3-dimethoxy benzenenbenzoyl chloridenanhydrous AlCl3= 11.051.05reaction temperature 05 reaction time 3 hproper demethylation reaction conditions were found asn2,4-dimethoxy-benzophenonenanhydrous AlCl3= 1(1.051.10)reaction temperature 2025 reaction time 3 hproper experimental conditions for sulfonation reaction were found asn(2-hydroxy-4-methoxy benzophenone)n(chlorosulfonic acid)= 11.05room temperature. The yield of 2-hydroxy-4-methoxy-5-sulfonic acid benzophenone was 72.35% based on 1,3-dimethoxy benzene and the purity was 99.21% as determined by HPLC. The molecular structures of 2-hydroxy-4-methoxy-5-sulfonic acid benzophenone and its intermediates were identified by 1H-NMR13C-NMR and FT-IR.

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