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原酸酯类除水剂介导的不对称二亚胺高效合成

Efficient Synthesis of Asymmetric Diimide Mediated by Primary Acid Ester Dehydrating Agent
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摘要 不对称二亚胺作为重要的配体,其工业化生产一直受限于反应选择性低和后处理复杂等问题。研究了2种有机除水剂(原乙酸三甲酯和原乙酸三乙酯)在二亚胺化合物合成反应中的作用效果,考察了除水剂种类、除水剂用量和温度对反应收率、选择性的影响。结果表明,2种除水剂的添加均能提高反应收率。其中,原乙酸三乙酯对反应的提升效果更为显著,在90℃、n(原乙酸三乙酯)∶n(单亚胺酮)=2.0条件下,成功将反应的核磁收率提高至92%,使后处理工艺得以简化。该研究不仅证实了在不对称二亚胺合成中,化学除水策略的可行性,更为工业化生产提供了高效的技术路线。 Asymmetric diimide,as an important ligand,has been limited in industrial production due to issues such as low reaction selectivity and complex post-processing.The effects of two organic water removal agents(trimethyl acetate and triethyl acetate)on the synthesis of diimide compounds were studied,and the effects of water removal agent type,dosage,and temperature on reaction yield and selectivity were investigated.The results indicate that the addition of both types of water removal agents can improve the reaction yield.Among them,triethyl acetate has a more significant effect on enhancing the reaction.Under the conditions of 90℃ and n(triethyl acetate):n(monoimine ketone)=2.0,the nuclear magnetic resonance yield of the reaction was successfully increased to 92%,simplifying the post-treatment process.This study not only confirms the feasibility of chemical water removal strategies in asymmetric diimide synthesis,but also provides an efficient technical route for industrial production.
作者 吕婵君 周凯静 庄严俊 肖飞彪 LU Chanjun;ZHOU Kaijing;ZHUANG Yanjun;XIAO Feibiao(Zhejiang Juhua Technology Center Co.,Ltd.,Quzhou,Zhejiang 324000)
出处 《化工生产与技术》 2025年第3期16-18,I0003,共4页 Chemical Production and Technology
关键词 不对称二亚胺 除水剂 原乙酸三乙酯 原乙酸三甲酯 asymmetric diimide water removal agent triethyl acetate trimethyl orthoacetate
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