5-二氯乙酰基-6-甲基-9-氧杂-1,5-二氮杂二环[4.3.0]壬烷的一锅法合成One-Pot Synthesis of 5-Dichloroacetyl-6-Methyl-9-Oxo-1,5-Diazabicyclo[4.3.0]Nonane
叶非,王滨,丁丽,付颖,岳明丽,曲丹丹
摘要(Abstract):
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。
关键词(KeyWords): 安全剂;二氯乙酰基二氮杂二环;一锅法合成;工艺条件
基金项目(Foundation): 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)
作者(Author): 叶非,王滨,丁丽,付颖,岳明丽,曲丹丹
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