乙基-4-（4-溴苯基）-1-（4-溴苯基）-2，6-双（4-氟苯基）-1，2，5，6-四氢吡啶-3-羧酸甲酯的合成及晶体结构

摘要

Using 4-fluorobenzaldehyde,4-bromoaniline and ethyl acetoacetate in the presence of [Bmim-G]+ [HSO4 ]- cat-alyst in ethanol at 40 ℃,the crude of ethyl-4-(4-bromophenyl)-1-(4-bromophenyl)-2,6-bis(4-fluorophenyl)-1,2,5, 6-tetra hydro-pyridine-3-carboxylate was synthesized.The crystal was obtained by recrystallization from EtOH (95%)and DMF.The structure was determined by IR,1 HNMR spectra and single crystal X-ray diffraction.The crystal structure belongs to monoclinic,space group P2 (1)/c with the cell parameters a =1.339 37 (12)nm,b =2.068 5(2)nm,c =1.272 63 (12 )nm,β= 106.934 0 (10 )°,Mr = 741.46,V = 3.372 9 (6 )nm3 ,D c = 1.460 Mg/m3 ,Z =4,μ(Mo Kα)=2.453 mm-1 ,F(000)=1 504.The structure was solved by direct methods and refined by full-matrix least squares method to the final final R 1 =0.189 4,R 2 =0.215 5.The largest differences in peak and hole of elcetron density are 916 nm-3 and 830 nm-3 .%4-氟苯甲醛、4-溴苯胺和乙酰乙酸乙酯在[Bmim-G]＋[HSO4]－催化下，于乙醇中40℃反应，得到乙基-4-（4-溴苯基）-1-（4-溴苯基）-2，6-双（4-氟苯基）-1，2，5，6-四氢吡啶-3-羧酸甲酯的粗品，经95％EtOH 与 DMF 混合溶剂重结晶得到其晶体．经 IR，1 HNMR 及单晶 X 射线法对化合物进行了表征，确认该晶体属于单斜晶系，空间群为P2（1）／c ，晶胞参数 a ＝1．33937（12）nm，b ＝2．0685（2）nm，c ＝1．27263（12）nm，β＝106．9340（10）°，Mr ＝741．46，V ＝3．3729（6）nm3，D c ＝1．460 Mg／m3，Z ＝4，μ（Mo Kα）＝2．453 mm－1，F（000）＝1504．最终的偏离因子为 R 1＝0．1894，R 2＝0．2155．最终差值电子密度的最高峰为916 nm－3，最低峰为830 nm－3．