卤素交换氟化合成氟乙酸甲酯  

Synthesis of Methyl Fluoroacetate by Halogen Exchange Fluorination

作　　者：吕早生[1] 胡亚[1] 赵金龙[1] 黄吉林[1] 武燕娟[1] 帅清昱[1] 

机构地区：[1]武汉科技大学化学工程与技术学院,湖北武汉430081

出　　处：《化学与生物工程》2012年第11期18-20,共3页Chemistry & Bioengineering

基　　金：高等学校博士学科点专项科研基金联合资助项目(20104219110003)

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%。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 %.

关 键 词：氟乙酸甲酯 卤素交换氟化 相转移催化 

分 类 号：O623.624[理学—有机化学]