1-甲基-3-苯基-5-对甲苯基-6,7,8,9,10,11,12,13,14,15-十氢-3H-环十二烷[d]吡唑并[3,4-b]吡啶的微波合成和结构表征  

Synthesis and crystal structure of 1-methyl-3-phenyl-5(p-tolyl) -6,7,8,9,10,11,12,13,14,15-decahydro-3 H-cyclododeca[d] pyrazolo[3,4-b]pyridine under Microwave Irradiation

作　　者：贾润红[1,2] 彭菊花[1] 姜波[2] 屠树江[2] 

机构地区：[1]连云港师范高等专科学校,江苏连云港222006 [2]江苏师范大学化学化工学院,江苏徐州221116

出　　处：《分子科学学报》2013年第1期37-40,共4页Journal of Molecular Science

基　　金：国家自然科学基金资助项目(200810102050);江苏省青蓝工程优秀骨干教师培养对象

摘　　要：标题化合物(C30H35N3)以4-甲基苯甲醛、环十二酮和3-甲基-1-苯基-1 H-吡唑-5-胺,在三氟乙酸和醋酸的作用下,经微波辐射合成得到.其结构通过单晶X射线衍射法确定,晶体属单斜晶系,空间群P21/c,相对分子质量Mr=437.61,晶胞参数a=1.089 26(11)nm,b=2.192 7(2)nm,c=1.049 54(14)nm,V=2.464 1(5)nm3,Z=4,晶胞密度Dc=1.180g/m3,吸收系数μ=0.069mm-1,单胞中电子的数目F(000)=944.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,最终的偏离因子为R=0.046 8,ωR=0.090 5.在晶体结构中新形成的吡啶环为共平面结构.The title compound （C30 Has Na） has been synthesized by the reaction of 4-methylbenzaldehyde, cyclododecanone and 3-methyl-l-phenyl-lH-pyrazol-5-amine in ethylene glycol under microwave irradiation. The structure was determined by single crystal X-ray diffraction. The crystal is monoclinic, space group P21/c, with Mr = 437. 61,a = 1. 089 26 （11） nm, b= 2. 192 7 （2） nm, c= 1. 049 54（14） nm, V=2. 464 1（5） nm3 ,Z=4,Dc=I. 180 g/cma,μ=0. 069 mm-1 ,F（000）=944. The structure was solve by direct methods and refined by full-mat rix least squares method to the final R = 0. 046 8,ωR=0. 090 5. X-ray analysis reveals that the newly formed pyridine ring in the crystal structure is a coplanar structure.

关 键 词：吡唑并[3 4-b]吡啶 合成 微波 晶体结构 

分 类 号：O626[理学—有机化学]