摘要
发展了一种基于(COCl)2/DMF原位反应制备的Vilsmeier-Haack试剂,催化酮肟Beckmann重排反应,通过探索优化反应条件发现以二氯甲烷为溶剂在室温条件下能以中等到优秀的产率合成各类酰胺及内酰胺。该反应体系可进一步用于克级规模酰胺或内酰胺的制备且无需柱层析分离纯化。另外,该方法中反应试剂与溶剂无需繁琐严格的无水处理,商品化购买的试剂与溶剂可直接使用。
A Vilsmeier-Haack reagent in situ generated from( COCl)2/DMF was developed to catalyze the Beckmann rearrangement reaction of ketoximes. By exploring and optimizing the reaction conditions,various amides and lactams could be obtained in moderate to excellent yield with methylene chloride as a solvent under mild conditions. The reaction system can be further applied for the preparation of gram-scale amides or lactams without separation and purification by column chromatography. In addition,in this method,the reaction reagent and the solvent didn’t require complicated and strict anhydrous treatment, and the commercially available reagents and solvents can be used directly.
作者
何晴媛
杨晓娜
吕瑞翠
邹亚萍
姚伟军
HE Qing-yuan;YANG Xiao-na;LV Rui-cui;ZOU Ya-ping;YAO Wei-jun(Department of Chemistry Zhejiang Sci-Tech University,Zhejiang Hangzhou 310018,China)
出处
《广州化工》
CAS
2019年第21期51-53,79,共4页
GuangZhou Chemical Industry