银催化的酰胺与N-甲基吡咯烷酮的sp~3C-N官能化反应

发布时间：2018-04-28 14:37

  本文选题：C-N键 + 交叉偶联反应　； 参考：《甘肃农业大学学报》2016年06期

【摘要】：【目的】研究交叉脱氢偶联(cross-dehydrogenative-coupling,CDC)反应机理及条件,寻求一种新的合成方法,最终实现酰胺与N-甲基吡咯烷酮sp3 C-N官能化反应.【方法】根据酰胺与N-甲基吡咯烷酮sp~3C-N官能化反应的反应机理和反应路径,对该反应可能的催化剂AgNO_3,FeCl_3,CuCl_2,CuCl,NiSO_4·6H_2O,Fe_2(SO_4)_3·xH_2O,SnCl_2·2H_2O,CuI,BiCl_3,CoCl_2·6H_2O及氧化剂TBHP,Ca(ClO)_2,K2S_2O_8等化合物进行了筛选,同时优化了反应条件.【结果】最佳催化剂为AgNO_3,氧化剂为K_2S_2O_8,最佳反应条件为温度75℃,反应时间4h,溶剂为体积分数50%的乙腈水溶液.合成了6种不同的酰胺衍生物,它们的产率在64%~75%之间.用核磁1 H谱和红外光谱鉴定合成新化合物的结构,表明这些化合物都是酰胺与N-甲基吡咯烷酮反应的主产物.【结论】该方法是一种实现交叉脱氢偶联(cross-dehydrogenative-coupling,CDC)反应的高效绿色的合成方法.
[Abstract]:[objective] to study the mechanism and conditions of cross-dehydrogenative coupling (CDCC) reaction, and to find a new synthesis method. Finally, the functionalization of amide with N-methylpyrrolidone sp3 C-N was realized. [methods] according to the reaction mechanism and path of sp~3C-N functionalization between amide and N-methylpyrrolidone, The possible catalysts for this reaction, AgNOSP, FeCl _ 3, CuCl _ 3, CuCl _ 2, CuCl _ 2 / Niso _ 4 H _ 2O _ 2 / C _ 2H _ 2O _ 2 / C _ 2H _ 2O _ 4 & S _ 2S _ 2O _ 4, were screened, and the reaction conditions were optimized. [results] the best catalyst is Agno _ 3, the oxidizer is K _ 2S _ 2O _ 8, the optimum reaction condition is 75 鈩，

本文编号：1815682