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

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。

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

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 simple,safe,mild and suitable to scale-up production.