N-[3-((3-二甲氨基)-1-氧-2-丙烯基)苯基]-N-乙基乙酰胺的合成改进  

Improvement and Synthesis of N-[3-((3-(Dimethylamino)-1-oxo-2-propenyl)phenyl]-N-ethyl Acetamide

作　　者：程青芳[1] 王启发[2] 包静炎 叶燕斌[1] 龚峰[1] 

机构地区：[1]淮海工学院化学工程系,江苏连云港222005 [2]淮海工学院海洋学院,江苏连云港222005

出　　处：《淮海工学院学报（自然科学版）》2007年第2期36-39,共4页Journal of Huaihai Institute of Technology:Natural Sciences Edition

基　　金：江苏省教育厅高校自然科学研究指导性计划项目(05KJD150024);淮海工学院自然科学基金资助项目(Z2006011)

摘　　要：以间硝基苯乙酮为起始原料,经过还原、酰化、乙基化和缩合合成了标题化合物。对此工艺的还原、酰化及乙基化反应进行了研究,通过铁粉-冰醋酸还原酰化一锅煮工艺,合成了间乙酰氨基苯乙酮,收率达85%。乙基化中,革除了无水操作,以氢氧化钾水溶液代替氢化钠,简化了操作,提高了安全性;以廉价的溴乙烷代替价格昂贵的碘乙烷作乙基化试剂,以丙酮代替四氢呋喃作溶剂,降低了成本,收率达98.5%。总收率达到77%,产品的质量分数大于99%。本工艺操作简便、安全,条件温和,易于工业化。N-[3-（ （3-（Dimethylamino）-1-oxo-2-propenyl） phenyl]-N-ethyl acetamide was synthesized from m-nitro acetophenone by reduction, acetylation, ethylation and condensation with an overall yield of 77%. Improvements for the technical methods of reduction, acetylation and ethylation were also studied. N-（3-acetylphenyl） acetamide was obtained through one pot procedure of reduction and acetylation with the yield of 85%. In ethylation reaction, sodium hydride was replaced by potassium hydroxide, acetone as solvent and bromoethane as ethylating reagent, which is convenient to operate and the cost was decreased. The yield of this step was 98.5%. The purity of title compound was over 99% by HPLC. This procedure was si e, safe, mild and suitable to scale-up production.

关 键 词：中间体 扎来普隆 乙基化 缩合 改进 

分 类 号：O623.738[理学—有机化学]