Synthesis and Crystal Structure Determination of 4’,9’,4”,9”-Tetra-t-Butyl- 1’,6’,1”,6”-Tetramethoxy-2,5-Dithia[3.3] Metabiphenylophane  被引量:1

Synthesis and Crystal Structure Determination of 4’,9’,4”,9”-Tetra-t-Butyl- 1’,6’,1”,6”-Tetramethoxy-2,5-Dithia[3.3] Metabiphenylophane

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作  者:Tetsuji Moriguchi Tatsuya Egami Daisuke Yakeya Venkataprasad Jalli Kenji Yoza Akihiko Tsuge Tetsuji Moriguchi;Tatsuya Egami;Daisuke Yakeya;Venkataprasad Jalli;Kenji Yoza;Akihiko Tsuge(Department of Applied Chemistry, Faculty of Engineering, Kyushu Institute of Technology, Kitakyushu, Japan;Japan Bruker AXS K.K.3-9, Yokohama, Japan)

机构地区:[1]Department of Applied Chemistry, Faculty of Engineering, Kyushu Institute of Technology, Kitakyushu, Japan [2]Japan Bruker AXS K.K.3-9, Yokohama, Japan

出  处:《Crystal Structure Theory and Applications》2016年第3期56-62,共7页晶体结构理论与应用(英文)

摘  要:The title compound 4’,9’,4”,9”-tetra-tert-butyl-1’,6’,1”,6”-tetramethoxy-2,5-dithia[3.3] metabiphenylophane was synthesized as a calixarene like large-sized metacyclophane from the corresponding 3,3’-bis(chloromethyl)-5,5’-bis(1,1-dimethylethyl)-2,2’-dimethoxy-1,1’-biphenyl and 3,3’-bis (mercaptomethyl)-5,5’-bis(1,1-dimethylethyl)-2,2’-dimethoxy-1,1’-biphenyl via an intermolecular condensation reaction. The compound was characterized using 1H NMR spectroscopy and mass spectrometry. Its exact conformational structure was determined via single crystal X-ray diffraction analysis. The compound has quite strained 1,2-alternate like structure because of its two high dihedral angled and rigid biphenyl parts in the crystal. The crystal includes the two isomers as two different 1,2-alternate like conformers, and the ratio of the two isomers is 78:22.The title compound 4’,9’,4”,9”-tetra-tert-butyl-1’,6’,1”,6”-tetramethoxy-2,5-dithia[3.3] metabiphenylophane was synthesized as a calixarene like large-sized metacyclophane from the corresponding 3,3’-bis(chloromethyl)-5,5’-bis(1,1-dimethylethyl)-2,2’-dimethoxy-1,1’-biphenyl and 3,3’-bis (mercaptomethyl)-5,5’-bis(1,1-dimethylethyl)-2,2’-dimethoxy-1,1’-biphenyl via an intermolecular condensation reaction. The compound was characterized using 1H NMR spectroscopy and mass spectrometry. Its exact conformational structure was determined via single crystal X-ray diffraction analysis. The compound has quite strained 1,2-alternate like structure because of its two high dihedral angled and rigid biphenyl parts in the crystal. The crystal includes the two isomers as two different 1,2-alternate like conformers, and the ratio of the two isomers is 78:22.

关 键 词:Crystal Structure Metabiphenylcyclophane 1 2-Alternate Conformers 

分 类 号:O62[理学—有机化学]

 

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