摘要
探索了以廉价的乙酰丙酸（1）、1,3-丙二胺（2）和二氯乙酰氯为原料,利用环合及酰基化反应,一锅法合成5-二氯乙酰基-6-甲基-9-氧杂-1,5-二氮杂二环[4.3.0]壬烷（4）。利用正交实验设计研究了反应过程中溶剂效应、反应温度、搅拌时间、和原料物质的量比对化合物产率的影响,确定了合成标题化合物的优化实验条件为：以甲苯为溶剂,反应温度为35-40℃,搅拌时间1 h,乙酰丙酸与1,3-丙二胺的物质的量比为1：1时产率达到66.3%。产物结构经红外光谱、核磁共振、元素分析和质谱进行表征。所用方法原料廉价易得、反应条件温和、操作简便,适于工业化生产。
A 5-dichloroacetyl-6-methyl-9-oxo-l,5-diazabicyclo[4.3.0]nonane one-pot synthetic route wasinvestigated via ring closure and acylation reactions using levulinic acid, 1,3-propanediamine anddichloroacetyl chloride as the starting materials. Yield affecting factors, such as solvents, reaction temperature,stirring time, and molar ratio of reactants, were studied under orthogonal experimental design. The optimumsynthetic condition were found as follows： toluene as solvent, reaction temperature 35--40℃, stirring time 1 hand the molar ratio of levulinic acid and 1,3-propanediamine 1：1. The yield could reach to 66.3%. Moreover, thestructure of the compound was characterized by IR, 1H-NMR, Z3C-NMR, MS, and elemental analysis. Thisstudy shows that the proposed synthetic route is simple with mild reaction conditions, and the raw materials arecheap and easy to obtain.
出处
《高校化学工程学报》
EI
CAS
CSCD
北大核心
2014年第2期342-345,共4页
Journal of Chemical Engineering of Chinese Universities
基金
国家自然科学基金(31101473)
黑龙江省教育厅科研项目(12521002)
哈尔滨市科技局科技创新人才基金(2012RFQXN015)
关键词
安全剂
二氯乙酰基二氮杂二环
一锅法合成
工艺条件
safener
dichloroacetyl diazabicyclo
one-pot synthesis
synthetic technology conditions
