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 ■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.
引文
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