摘要
将磺酰脒铑[Rh_(2)(Msip)_(4)]和70%叔丁基过氧化氢水溶液(T-HYDRO)组成的催化氧化体系应用于芳基叔胺与酰(亚)胺的C-N交叉脱氢偶联反应,合成了一系列Mannich碱,通过^(1)HNMR、^(13)CNMR对其结构进行了表征,并对合成条件进行了优化。结果表明,在Rh_(2)(Msip)_(4)用量为0.5%(摩尔分数)、T-HYDRO用量为2.0 eq.、芳基叔胺与酰(亚)胺物质的量比为2∶1、溶剂为乙醇、反应温度为60℃的最佳条件下,目标化合物产率最高达到90%。
We synthesized a series of Mannich bases by C-N cross dehydrogenation coupling reaction of tertiary anilines and amides(or amides-imide)in a catalytic oxidation system consisting of sulfonamidine dirhodium[Rh_(2)(Msip)_(4)]and 70%tert-butyl hydroperoxide solution(T-HYDRO).Moreover,we characterized the structures of the target compounds by ^(1)HNMR and ^(13)CNMR,and optimized the synthetic conditions.The results show that the yield of the target compound can reach as high as 90%under the optimal conditions as follows:the Rh_(2)(Msip)_(4) dosage of 0.5%(molar fraction),the T-HYDRO dosage of 2.0 eq.,the molar ratio of tertiary anilines to amides(or amides-imide)of 2∶1,ethanol is adopted as the solvent,and the reaction temperature of 60℃.
作者
阿迪拉·阿木提
徐秀娟
李佳佳
阿不都热合曼·乌斯曼
AMUTI Adila;XU Xiujuan;LI Jiajia;WUSIMAN Abudureheman(School of Chemistry and Chemical Engineering,Xinjiang Normal University,Urumqi 830054,China)
出处
《化学与生物工程》
CAS
2022年第10期46-49,共4页
Chemistry & Bioengineering
基金
新疆师范大学优秀青年教师科研启动基金项目(XJNU202013)。