| 3-溴-2-氟苯甲酸的合成 |
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| 引用本文： | 赵昊昱,周鹏鹏.3-溴-2-氟苯甲酸的合成[J].化学世界,2013,54(5):297-300. |
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| 作者姓名： | 赵昊昱 周鹏鹏 |
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| 作者单位： | 常州工程职业技术学院化工系,江苏常州,213164 |
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| 基金项目： | 江苏省教育厅高校科研成果产业化推进拨款项目，江苏省教育厅高校“青蓝工程”中青年学术带头人培养对象项目 |
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| 摘 要： | 以2-氨基-6-氟苯腈为原料,经溴化、水解和重氮化脱氨基反应合成3-溴-2-氟苯甲酸,产物的含量为99.20%(HPLC),总摩尔产率约38%。产物结构通过MS和1 H NMR验证。其中溴化反应的最佳条件为n(2-氨基-6-氟苯腈)∶n(NBS)=1∶1.05,n(2-氨基-6-氟苯腈)∶n(DMF)=1∶6,反应温度为5℃;水解反应的最佳反应条件为n(2-氨基-5-溴-6氟苯腈)∶n(NaOH)=1∶1.5,水解时间为8h,温度控制在回流状态下。该法具有生产成本低、反应条件温和、易于工业化生产的优点。
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| 关 键 词： | 2-氨基-6-氟苯腈 3-溴-2-氟苯甲酸 合成 |
Synthesis of 3-Bromo-2-fluorobenzoic Acid |
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| ZHAO Hao-yu,ZHOU Peng-peng.Synthesis of 3-Bromo-2-fluorobenzoic Acid[J].Chemical World,2013,54(5):297-300. |
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| Authors: | ZHAO Hao-yu ZHOU Peng-peng |
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| Affiliation: | (Changzhou Institute of Engineering Technology,Department of Chemical Engineering,Jiangsu Changzhou 213164,China) |
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| Abstract: | 3-Bromo-2-fluorobenzoic acid with an overall yield of 38% and purity of 99.202%(HPLC).was synthesized from 2-amino-6-fluorobenzonitrile by bromination,hydrolysis,diazotization and deamination.The structure of the product was confirmed by MS and 1H NMR.The optimized conditions of bromination were: n(2-amino-6-fluorobenzonitrile)∶n(NBS)=1∶1.05,n(2-amino-6-fluorobenzonitrile)∶n(DMF)=1∶6,temperature at 5℃.The optimized conditions of hydrolysis were: n(2-amino-5-bromo-6-fluorobenzonitrile)∶n(NaOH)=1∶1.5,8 h,under reflax.This method has the advantages of low cost and mild reaction conditions,and it is suitable for production in industrial scale. |
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| Keywords: | 2-amino-6-fluorobenzonitrile 3-bromo-2-fluorobenzoic acid synthesis |
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