摘要
以甲基磺酸和碳酸镉为原料,采用普通溶液法制备甲基磺酸镉(Ⅱ),其产物为白色结晶固体。采用红外、核磁、热重、扫描电镜和X射线单晶衍射多种方法对化合物进行表征。结果表明:甲基磺酸镉含有两个结晶水,热稳定性好,属于三斜晶系,■空间群;晶胞参数a=0.4785(5)nm,b=0.6101(5)nm,c=0.8232(5)nm,α=87.137(5)°,β=84.461(5)°,γ=85.614(5)°,V=0.2383(3)nm^3,Z=1。以N1-甲基3,4-二氢嘧啶酮的合成为探针反应,考察了甲基磺酸镉对Biginelli反应的催化性能。在无溶剂、绿色条件下,产品收率达90.1%,重复使用三次后。产品收率仍可以达到80.3%。最后,对甲基磺酸镉连续催化后,催化活性略有下降的原因进行了分析。
Cadmium(Ⅱ)methanesulfonate was prepared from methanesulfonic acid and cadmium carbonate using the common solution method,and the product is white crystalline solid.It was characterized by IR,NMR,TG,SEM and X-ray single crystal diffraction techniques.The results show cadmium methanesulfonate contains two crystal water molecules and has good thermal stability.It is triclinic,belonged to the P1 space group with a =0.4785(5)nm, b =0.6101(5)nm, c =0.8232(5)nm,α=87.137(5)°,β=84.461(5)°,γ=85.614(5)°, V =0.2383(3)nm 3, Z =1.The catalytic activity of cadmium methanesulfonate was investigated by using the synthesis of N1-methyl 3,4-dihydropyrimidinone as a probe reaction.The yield of the product reaches 90.1%under solvent-free and green conditions.The yield of the product was as high as 80.3%even if the catalyst was reused after three cycles.At last,the reasons for the slight decrease in catalytic activity after continuous catalysis of cadmium methanesulfonate were analyzed.
作者
宋志国
张顺
向刚伟
王敏
SHONG Zhi-guo;ZHANG Shun;XIANG Gang-wei;WANG Min(Center of Experimental Management,Bohai University,Jinzhou 121013,China;College of Chemistry&Chemical Engineering,Bohai University,Jinzhou 121013,China;The First Produce Department of PetroChina Sichuan Petrochemical Co.,Ltd.,Chengdu 611930,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2019年第5期954-959,共6页
Chemical Research and Application
基金
辽宁省高等学校优秀人才支持计划(LJQ2015002)资助
辽宁省自然科学基金项目(2015020201)资助
国家自然科学基金项目(21406016)资助
关键词
甲基磺酸镉
表征
BIGINELLI反应
催化
cadmium(Ⅱ)methanesulfonate
characterization
Biginelli reaction
catalysis