| 卤素交换氟化合成氟乙酸甲酯 |
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| 引用本文： | 吕早生,胡亚,赵金龙,黄吉林,武燕娟,帅清昱. 卤素交换氟化合成氟乙酸甲酯[J]. 化学与生物工程, 2012, 29(11): 18-20 |
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| 作者姓名： | 吕早生 胡亚 赵金龙 黄吉林 武燕娟 帅清昱 |
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| 作者单位： | 武汉科技大学化学工程与技术学院,湖北武汉,430081 |
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| 基金项目： | 高等学校博士学科点专项科研基金联合资助项目 |
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| 摘 要： | 以氯乙酸甲酯和喷雾干燥氟化钾(SD-KF)为原料、N,N-二甲基甲酰胺(DMF)为溶剂、乙酰胺为助溶剂、四苯基溴化膦(Ph4PBr)为催化剂合成了氟乙酸甲酯。确定了反应的最适条件:反应体系为11.5mL DMF+4.5g乙酰胺+1.0g Ph4PBr、n(KF)∶n(氯乙酸甲酯)为2.5∶1、反应温度为130℃、反应时间为4h,在此条件下,氯乙酸甲酯转化率为90.5%,氟乙酸甲酯的收率为82.3%。
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| 关 键 词： | 氟乙酸甲酯 卤素交换氟化 相转移催化 |
Synthesis of Methyl Fluoroacetate by Halogen Exchange Fluorination |
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| L Zao-sheng , HU Ya , ZHAO Jin-long , HUANG Ji-lin , WU Yan-juan , SHUAI Qing-yu. Synthesis of Methyl Fluoroacetate by Halogen Exchange Fluorination[J]. Chemistry & Bioengineering, 2012, 29(11): 18-20 |
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| Authors: | L Zao-sheng HU Ya ZHAO Jin-long HUANG Ji-lin WU Yan-juan SHUAI Qing-yu |
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| Affiliation: | L(U) Zao-sheng , HU Ya , ZHAO Jin-long , HUANG Ji-lin , WU Yan-juan , SHUAI Qing-yu |
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| Abstract: | Methyl fluoroacetate was prepared by halogen exchange fluorination of methyl chloroacetate with spray-dried KF,using DMF as solvent, acetamide as co-solvent and Ph4 PBr as catalyst. The optimal reaction conditions were obtained as follows.the reaction system consisted of 11.5 mL DMF,4.5 g acetamide and 1.0 g Ph4PBr, molar ratio of KF to methyl chloroacetate was 2.5 ： 1,reaction temperature was 130 ℃ and reaction time was 4 h. Under above conditions,the conversion rate of methyl chloroacetate was 90. 5% and the yield of methyl fluoroacetate was 82.3 %. |
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| Keywords: | methyl fluoroacetate halogen exchange fluorination phase transfer catalysis |
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