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有机化学
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有机化学 ›› 2011, Vol. 31 ›› Issue (04): 528-532. 上一篇    下一篇

研究论文

水杨醛缩2-茚(芴)基乙胺席夫碱的合成及其晶体结构

李邦玉*,1,2，姚英明2，王耀荣2，张勇2，沈琪*,2，魏入铎1   

  1. (1苏州市职业大学应用化学研究所 苏州 215104)
    (2苏州大学材料与化学化工部 苏州 215123)
  • 收稿日期:2010-07-28 修回日期:2010-10-21 发布日期:2010-11-30
  • 通讯作者: 李邦玉 E-mail:lby716103@163.com

Synthesis, Crystal Structures of 3,5-Bi-tert-butylsalicylicylidene-2- indenyl(fluorenyl)ethylamine Schiff-Bases

Li Bangyu*,1,2 Yao Yingming2 Wang Yaorong2 Zhang Yong2 Shen Qi*,2 Wei Ruduo1   

  1. (1 Institute of Applied Chemistry, Suzhou Vocational University, Suzhou 215104)
    (2 Key Laboratory of Organic Synthesis of Jiangsu Province, College of Chemistry, Chemical Engineering and Materials Science, Suzhou University, Suzhou 215123)
  • Received:2010-07-28 Revised:2010-10-21 Published:2010-11-30

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被引次数

2

茚基(芴基)锂与2-溴乙胺氢溴酸盐在乙醚中按2∶1物质的量比反应, 分别得到2-茚基(芴基)乙胺氢溴酸盐(1)和3, 1和3再与水杨醛缩合, 分别得到水杨醛缩2-茚基(芴基)乙胺席夫碱2和4. 通过1H NMR, IR, MS和元素分析等手段对产物进行了表征, X射线分析确定了2, 4的晶体结构. 其中化合物2属于单斜晶系, P21/c空间群, a＝0.9771(2) nm, b＝1.9561(4) nm, c＝1.1901(3) nm, β＝99.955(5)°, Mr＝375.53, V＝2.2404(8) nm3, Dc＝1.113 g/cm3, Z＝4, F(000)＝816, μ＝0.066 mm－1, R1＝0.0769, wR2＝0.1625. 化合物4属于三斜晶系, P空间群, a＝0.9688(3) nm, b＝0.9699(3) nm, c＝1.3535(5) nm, α＝95.280(7)°, β＝105.394(11)°, γ＝90.987(12)°, Mr＝425.59, V＝1.2197(8) nm3, Dc＝1.159 g/cm3, Z＝2, F(000)＝460, μ＝0.069 mm－1, R1＝0.0589, wR2＝0.1312..

关键词: 茚, 芴, 水杨醛, 席夫碱, 合成, 晶体结构

Reaction of indenyl lithium or fluorenyl lithium with 2-bromoethylamine hydrobromide gave two new intermediates 1 and 3 respectively, which were then condensed with 3,5-di-tert-butylsalicylalde- hyde to afford two new Schiff bases 2 and 4 respectively. These compounds were characterized by elemental analysis, IR spectra and X-ray structural determination. The crystal of the compound 2 belongs to monoclinic, space group P21/c with cell parameter a＝0.9771(2) nm, b＝1.9561(4) nm, c＝1.1901(3) nm, β＝99.955(5)°, Mr＝375.53, V＝2.2404(8) nm3, Dc＝1.113 g/cm3, Z＝4, F(000)＝816, μ＝0.066 mm－1, R1＝0.0769 and wR2＝0.1625. The crystal of the compound 4 belongs to triclinic, P space group, a＝0.9688(3) nm, b＝0.9699(3) nm, c＝1.3535(5) nm, α＝95.280(7)°, β＝105.394(11)°, γ＝90.987(12)°, Mr＝425.59, V＝1.2197(8) nm3, Dc＝1.159 g/cm3, Z＝2, F(000)＝460, μ＝0.069 mm－1, R1＝0.0589 and wR2＝0.1312.

Key words: indene, fluorene, salicylaldehyde, Schiff-base, synthesis, crystal structure