4-(2,5-二甲基-3,4-二乙酰基)-1-吡咯基苯甲酸的合成及其晶体结构  

Synthesis and Crystal Structure of 4 (2,5 dimethyl 3,4 diacetyl) 1 pyrrolyl Benzoic Acid

作　　者：朱洪友[1] 谢小光[1] 杨宗璐[1] 刘复初[1] 郁开北[2] 

机构地区：[1]云南大学化学系 [2]中国科学院成都分院分析测试中心

出　　处：《人工晶体学报》1998年第4期51-55,共5页Journal of Synthetic Crystals

基　　金：云南省应用基础研究基金

摘　　要：在强酸性介质中，３，４－二乙酰基－２，５－己二酮与对氨基苯甲酸作用，满意地得到了４（２，５二甲基３，４二乙酰基）１吡咯基苯甲酸，用ＩＲ、１ＨＮＭＲ、高分辩质谱等对其进行了表征，用Ｘ射线衍射测定了晶体结构。该晶体属三斜晶系，Ｐ１空间群，ａ＝０．８０９５０（１０）ｎｍ，ｂ＝０．８１９１０（１０）ｎｍ，ｃ＝１．１９００（２）ｎｍ，α＝１０１．６００（１０）°，β＝９８．８２０（１０）°，γ＝１０４．９６０（１０）°，Ｚ＝２，Ｄｃ＝１．３６４×１０３ｋｇ／ｍ３。拟合了苯环平面和吡咯环平面的平面方程，并求出两平面之间的二面角为６８．１１°。The 4 (2,5 dimethyl 3,4 diacetyl) 1 pyrrolylbenzoic acid were synthesized in satisfactory yield through the reaction of 3,4 diacetyl 2,5 hexanedione with 4 aminobenzoic acid in strong acidity medium.The structure of the title compound was characterized by IR、 1H NMR、high resolution MS,and also determined by X ray single crystal diffraction analysis.The crystal is triclinic with space group P 1-.The unit cell parameters are as follow: a =0.80950(10)nm, b =0.81910(10)nm, c =1.1900(2)nm, α =101.600(10)°, β =98.820(10)°, γ =104.960(10)°, Z =2, D c=1.364×10 3kg/m 3.The plane equation of benzene ring and pyrrol ring were evaluated and their dihedral angle is 68.11°。

关 键 词：吡咯基苯甲酸 3.4-二乙酰基-2.5-己二酮 晶体结构 溶液晶体生长 

分 类 号：O782.1[理学—晶体学] O76