离子液体中8-(2-甲氧基苯基)-3,5-二[(E)-1-(2-甲氧基苯基)亚甲基]-1,2,3,5,6,7-六氢二环戊二烯并[b,e]吡啶的合成与晶体结构

Synthesis and crystal structure of 8-(2-methoxyphenyl)-3,5-di[(E)-1-(2-methoxyphenyl)-methylidene]-1,2,3,5,6,7-hexahydrodicyclopenta[b,e]pyridine in ionic liquids

在离子液体([BPY]BF4)存在下,由2-甲氧基苯甲醛、环戊酮和醋酸铵一锅法合成,并经N,N-二甲基甲酰胺(DMF)与95%的乙醇混合溶剂重结晶得到化合物8-(2-甲氧基苯基)-3,5-二[(E)-1-(2-甲氧基苯基)亚甲基]-1,2,3,5,6,7-六氢二环戊二烯并[b,e]吡啶的晶体.其结构通过IR,1 HNMR,13 CNMR进行表征,用X射线单晶衍射法测定该化合物的晶体结构.结果表明,晶体属三斜晶系,P1空间群,a=1.103 66(14)nm,b=1.167 47(17)nm,c=1.229 54(19)nm,α=69.78(0)°,β=66.34(0)°,γ=81.53(0)°,Mr=501.60,V=1.361 59(84)nm3,Z=2,μ(Mo Kα)=0.077mm-1,F(000)=532.最终偏离因子R=0.183 5,Rw=0.221 0.化合物分子中,原子C1,C5,C6,C7,C11和N1形成一个六元吡啶环.

The title compound 8‐（2‐methoxyphenyl）‐3 ,5‐di[（E）‐1‐（2‐methoxyphenyl）‐methylidene]‐1 ,2 ,3 ,5 ,6 ,7‐hexahydrodicyclopenta[b ,e]pyridine was obtained by the reaction of 2‐methoxy benzaldehyde ,cyclopentanone and ammonium acetate in ionic liquid （[BPY]BF4 ） and by recrystallization from EtOH（95% ） and DMF .The structure of the compound was characterized by IR ,1 HNMR ,13CNMR and X‐ray single crystal diffraction .The results show that the crystal belongs to triclinic system ,P1 space group with a=1.103 66（14） nm ,b=1.167 47（17） nm ,c=1.229 54（19） nm ,α= 69.78（0）° ,β= 66.34（0）° ,γ= 81.53（0）° ,Mr = 501.60 ,V = 1.361 59（84） nm3 ,Z= 2 ,μ（Mo Kα）=0.077 mm -1 ,F（000）=532 ,R=0.183 5 ,Rw =0.221 0 .X‐ray analysis reveals that atoms C1 ,C5 , C6 ,C7 ,C11 and N1 form a six‐membered pyridine ring .