SYNTHESIS, SOLID-STATE STRUCTURE, AND REDUCTION OF 1,1-DICHLORO-2,3,4,5-TETRAMETHYLSILOLE

被引:95
作者
BANKWITZ, U [1 ]
SOHN, H [1 ]
POWELL, DR [1 ]
WEST, R [1 ]
机构
[1] UNIV WISCONSIN,DEPT CHEM,MADISON,WI 53706
关键词
SILICON; ZIRCONIUM; LITHIUM; SILOLE; CRYSTAL STRUCTURE; DIANION;
D O I
10.1016/0022-328X(95)00333-L
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The previously unknown 1,1-dichloro-2,3,4,5-tetramethyl-1-silacyclopenta-2,4-diene (3) was prepared in a three-step synthesis starting from zirconocene dichloride, 2-butyne, and n-butyllithium via bis(cyclopentadienyl)-2,3,4,5-tetramethyl-1-zirconacyclopenta-2,4-diene (1) and 1,4-diiodo-1,2,3,4-tetramethylbuta-1,3-diene (2). 3 was characterized by NMR spectroscopy and single-crystal X-ray diffraction. Reaction of the new silole 3 with 4 equivalents of lithium in THF gives the corresponding dianion 4. H-1-, C-13-, and Si-29-NMR chemical shifts of 4 compared with 3 indicate some aromatic character for the ionic species. Trapping of 4 with Me(3)SiCl gives 1,1-bis(trimethylsilyl)-2,3,4,5-tetramethylsilole (5) in quantitative yield.
引用
收藏
页码:C7 / C9
页数:3
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