高纯度N-甲基邻氟苯胺的合成新工艺  

New Synthesis Process of High Purity N-Methyl-2-fluoroaniline

作　　者：李爱军[1,2] 史帅帅 LI Ai-jun;Sill Shuai-shuai(College of Chemical and Pharmaceutical Engineering;State Key Laboratory Breeding Base-Key Laboratory of Molecular Chemistry for Drug of Hebei Province, Hebei University of Science and Technology, Shijiazhuang 050018, China)

机构地区：[1]河北科技大学化学与制药工程学院,河北石家庄050018 [2]河北科技大学河北省药用分子化学重点实验室-省部共建国家重点实验室培育基地,河北石家庄050018

出　　处：《化学试剂》2018年第7期699-702,共4页Chemical Reagents

摘　　要：N-甲基邻氟苯胺是重要的精细化工、农药、医药中间体,对N-甲基邻氟苯胺的合成新工艺进行研究。以邻氟苯胺为起始原料,回流下与过量的甲酸进行甲酰化得到N-邻氟苯基甲酰胺,收率95.3%。得到的N-邻氟苯基甲酰胺与甲磺酸甲酯在甲醇钠的作用下于50℃甲基化得到N-甲基-N-邻氟苯基甲酰胺,收率94.4%。N-甲基-N-邻氟苯基甲酰胺在盐酸-甲醇溶液中60℃水解5 h得到目标产物。在优化的反应条件下,总收率为83.0%,纯度99.5%。该方法操作简单、原料易得、避免了精馏分离,适合工业化生产。N-Methyl-2-fluoroaniline is an important intermediate of fine chemical,pesticide and medicine,a new method for the synthesis of N-methyl-2-fluoroaniline was investigated. N-2-fluorophenylformamide was obtained from 2-fluoroaniline as starting material via the process of formylation of excess formic acid under reflux,the yield was 95. 3%. N-methyl-N-2-fluorophenylformanide was obtained by methylation of methyl methanesulfonate and N-2-fluorophenyformamide at 50 ℃ under the action of sodium methoxide,the yield was 94. 4%.N-methyl-N-2-fluorophenylformanide was obtained in hydrochloric acid-methanol solution at 60% hydrolysis for 5 h,and the target product was obtained.Under the optimal conditions,the total yield was 83. 0% and the purity was 99. 5%.The synthetic process has simple operations,the raw material is easily available,distillation separation is avoided and is suitable for industrial production.

关 键 词：N-甲基邻氟苯胺 邻氟苯胺 甲酰化 合成 

分 类 号：TQ457.2[化学工程—农药化工]