9,9-双(丙酸丁酯基)芴的合成及晶体结构

实验以芴为原料、丙烯酸丁酯为烷基化试剂,一步反应合成了9,9-双(丙酸丁酯基)芴,收率达到90%。在乙醇溶剂中培养出单晶,通过X射线单晶结构分析法测定了分子结构和晶体结构。晶体属于单晶系,P2(1)/c空间群,晶胞参数为:a=12.912 2(11),b=10.973 9(10),c=1.746 8×10~(-9)(15)m,β=90.252(2),V=2.475 2×10~(-29)(4)m~3,Z=4,D_c=1.134 g/cm~3,μ(Mo K_α)=0.075 mm~(-1),F(000)=912,R=0.0651,wR=0.147 5。晶体结构分析表明,芴环上两个苯环和五元环接近共平面,侧链的两个酯基都是无序的,且该分子由分子键的CH…O氢键,连接成中心对称的二聚体结构,再由范德华力作用组成三维网状结构。

SYNTHESIS AND CRYSTAL STRUCTURE OF 9,9-BIS(BUTHOXYCARBONYLETHYL)FLUORENE

Synthesis of 9,9-bis(buthoxycarbonylethyl)fluorene with butyl acrylate as alkylation reagent and fluorene as starting material has been performed.And the field of 9,9-bis(buthoxycarbonylethyl) fluorine was 90%.The crystal structure was determined by the X-ray diffraction method.The crystal belongs to monoclinic,space group P2(1)/c with a= 12.912 2(11),b= 10.973 9(10),c = 1.746 8×10~(-9)(15) m,β=90.252(2),V=2.475 2×10~(-29)(4) m~3,Z=4,D_c= 1.134 g/cm~3,μ(Mo K_α= 0.075 mm~(-1),F(000) =912,R= 0.065 wR = 0.147 5.X-ray analysis reveals that the three fused rings of the fluorene system are almost coplanar and the two ester groups are nearly perpendicular to the fused-ring system,weak CH…O hydrogen-bonding connects the molecule into centrosymmetric dimmers.