2,5-二(2,4-二乙基苯甲酰基)对苯二甲酸的合成及晶体结构

Synthesis and crystal structure of 2,5-bis(2,4-die thylbenzoyl) terephthalic acid

以均苯四甲酸酐与间二乙苯为原料,合成了未见文献报道的2,5-二(2,4-二乙基苯甲酰基)对苯二甲酸,利用溶剂挥发法得到该化合物的单晶.同时对其进行了元素分析、核磁共振表征和X射线单晶衍射分析.晶体结构分析结果表明:该晶体属于三斜晶系,P-1空间群,a=0.545 1(11)nm,b=0.751 1(15)nm,c=1.584 4(3)nm,α=84.45(3)°,β=85.37(3)°,γ=85.86(3)°,Dc=1.258 g/cm3,Z=2,F(000)=258,μ=8.7×10-8nm-1,最终偏差因子分别为R=0.147 3,wR=0.209 7.分子之间通过相邻分子间形成的O—H…O氢键相连,分子间和内部的氢键使得晶体结构稳定性增强.

The compound of 2,5-bis （2,4-diethylbenzoyl） terephthalic acid （BDTA） was first synthesized by the reaction of pyromellitic dianhydride with m-diethyl benzene, of which the single crystal was obtained by slowly evaporation of solvent. The structure of BDTA was confirmed by elemental analysis, I H-NMR as well as single crystal X-ray diffraction analysis. And X-ray analysis reveals that the crystal belongs to triclinic, space group P - 1 with a = 0.545 1（11） nm, b=0.751 1 （15） nm, c=1.5844 （3） nm, α =84.45（3）°, β=85.37（3）°,γ = 85.86（3）°, Dc =1.258 g/cm^3, Z=2, F（000） =258, μ=8.7 × 10^-8nm^-1, the final R =0. 147 3 and wR = 0.209 7. In the crystal, BDTA molecules are linked by intermolecular O-H…O hydrogen bonds to form a linear structure. All the intra-and inter-molecular hydrogen bonds may be effective in the stabilization of the crystal structure.