3-甲基-1,6-二苯基-4-(噻吩-2-基)-1H-吡唑并[3,4-b]吡啶-5-甲腈的绿色合成和结构表征

Green synthesis and crystal structure of 3-methyl-1.6-diphenyl-4-(thiophen-2-yl)-1H-pyrazolo[3,4-b]pyridine-5-carbonitrile

标题化合物(C24H16N4S)以噻吩-2-甲醛、苯甲酰乙腈和3-甲基-1-苯基-1H-吡唑-5-胺为原料,在离子液体[bmim]Br溶剂中,在80℃搅拌合成得到.其结构通过单晶X射线衍射法确定,晶体属于三斜晶系,空间群P-1,相对分子质量Mr=392.47,晶胞参数a=0.936 12(8)nm,b=1.030 63(12)nm,c=1.166 24(16)nm,V=0.968 53(19)nm3,Z=2,晶胞密度Dc=1.346g/cm3,吸收系数μ=0.185mm-1,单胞中电子的数目F(000)=408.晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子R=0.058 5,wR=0.133 7.在晶体结构中新形成的吡啶环与吡唑环近似于共平面结构.

The title compound（C24H16N4S）has been synthesized by the three-component reaction of thiophene-2-carbaldehyde,3-oxo-3-phenylpropanenitrile and 3-methyl-1-phenyl-1 H-pyrazol-5-amine in ionic liquid[bmim]Br.The structure was determined by single crystal X-ray diffraction analysis.It is triclinic,space group P-1,with Mr=392.47,a=0.936 12（8）nm,b=1.030 63（12）nm,c=1.166 24（16）nm,V=0.968 53（19）nm3,Z=2,Dc=1.346g/cm3,μ=0.185mm-1,F（000）=408.The structure was solved by direct methods and refined by full-matrix least squares method to the final R=0.058 5,wR=0.133 7.X-ray analysis reveals that the newly formed pyridine ring in the crystal structure is a coplanar structure with pyrazole ring fused.