高等学校化学学报 ›› 2011, Vol. 32 ›› Issue (6): 1305.

• 研究论文 • 上一篇    下一篇

3-茂铁基-5-芳基-1-苯磺酰基二氢吡唑衍生物的合成及晶体结构

李春艳2,3, 卓继斌2, 谢莉莉1,2, 李恒东2, 王文峰2, 袁耀锋1,2   

  1. 1.  福州大学光催化福建省重点实验室\|省部共建国家重点实验室培育基地,    福州 350002;
    2.  福州大学化学化工学院,  福州 350108;
    3.  福建医科大学药学院, 福州 350108
  • 收稿日期:2010-07-23 修回日期:2010-10-08 出版日期:2011-06-10 发布日期:2011-05-10
  • 通讯作者: 袁耀锋 E-mail:yaofeng_yuan@fzu.edu.cn
  • 基金资助:

    国家自然科学基金(批准号: 20772016), 福建省自然科学基金(批准号: 2009J05028, 2010J01036 ), 福建省科技计划重点项目(批准号: 2009H0021), 福建省教育厅科研资助项目(批准号: JA07017)和福州大学光催化省部共建国家重点实验室培育基地开放课题(批准号: K-081009)资助.

Synthesis and Crystal Structure of 3-Ferrocenyl-5-aryl-1-benzenesulfonyl Dihydropyrazole Derivatives

LI Chun-Yan2,3, ZHUO Ji-Bin2, XIE Li-Li1,2, LI Heng-Dong2, WANG Wen-Feng2, YUAN Yao-Feng1,2*   

  1. 1.  State Key Laboratory Breeding Base of Photocatalysis, Fuzhou University, Fuzhou 350002, China;
    2.  College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350108, China;
    3.  Faculty of Pharmacy, Fujian Medical University, Fuzhou, 350108, China
  • Received:2010-07-23 Revised:2010-10-08 Online:2011-06-10 Published:2011-05-10
  • Contact: YUAN Yao-Feng E-mail:yaofeng_yuan@fzu.edu.cn
  • Supported by:

    国家自然科学基金(批准号: 20772016), 福建省自然科学基金(批准号: 2009J05028, 2010J01036 ), 福建省科技计划重点项目(批准号: 2009H0021), 福建省教育厅科研资助项目(批准号: JA07017)和福州大学光催化省部共建国家重点实验室培育基地开放课题(批准号: K-081009)资助.

摘要: 以α,β-不饱和酮为起始原料,设计合成了2种二茂铁取代的4,5-二氢吡唑化合物,用IR、1H NMR、对其结构进行了表征,并采用X射线单晶衍射测定后确认化合物3a、3b的晶体和分子结构,化合物3a(C25H22FeN2SO2)属于正交晶系(Orthorhombic),P2(1)2(1)2(1)空间群,晶胞参数:a = 0.59466(12) nm,b = 1.9402(8) nm,c = 3.1274(6) nm,α = 90.00°,β = 90.00°,γ = 90.00°,Z = 4,F(000) = 1280,DC = 1.442 g/cm3,μ = 0.817 nm-1.该化合物通过分子间的氢键沿a轴延伸形成一维链状结构.化合物3b(C25H21FeN2SO2Br)属于单斜晶系(Monoclinic),P2(1)/c空间群,晶胞参数:a = 1.3087(3) nm,b = 0.9844(2) nm,c = 1.7752(4) nm,α = 90.00°,β = 99.42(3)°,γ = 90.00°,Z = 4,F(000) = 1112.0,DC = 1.617 g/cm3,μ = 2.558 nm-1.该化合物中每一个分子与其邻近的3个分子连接,以氢键的作用缔合在一起,以此延伸,形成稳定的超分子化合物.

关键词: 二茂铁基衍生物, 二氢吡唑, 分子间氢键, 分子组装

Abstract: Two Novel 3-diferrocenyl dihydropyrazole derivatives were synthesized from corresponding α,β-unsaturated ketones. The structures of these compounds were characterized by IR, 1H NMR spectra and X-ray single crystal diffraction. The crystal structure of compound 3a belongs to the orthorhombic,space group P2(1)2(1)2(1) with the lattice parameters a = 0.59466(12) nm,b = 1.9402(8) nm,c = 3.1274(6) nm,α = 90.00°,β = 90.00°,γ = 90.00°,Z = 4,F(000) = 1280,DC = 1.442 g/cm3,μ = 0.817 nm-1. Its crystal structure showed that chain-like one-dimentional structure was formed along a axis by the intermolecular hydrogen bonds.The compound 3b belongs to the monoclinic, space group P2(1)/c,and its lattice parameters are as follows: a = 1.3087(3) nm,b = 0.9844(2) nm,c = 1.7752(4) nm,α = 90.00°,β = 99.42(3)°,γ = 90.00°,Z = 4,F(000) = 1112.0,DC = 1.617 g/cm3,μ = 2.558 nm-1. The intermolecular hydrogen bonds between the sulfonyl oxygen and nonsubstituted cyclopentadienyl (Cp) hydrogen and bromobenzene hydrogen led to the formation of stable supermolecular structure of one 3b with three otherwise 3b molecules.

Key words: Ferrocenyl derivatives, Dihydropyrazole, Intermolecular hydrogen bond, Molecular assembly

TrendMD: