PREPARATION OF THE 1,2-DI-TERT-BUTYLCYCLOPENTADIENYL ANION AND A TRANSITION-METAL DERIVATIVE - CRYSTAL-STRUCTURE OF 1,1',2,2'-TETRA-TERT-BUTYLFERROCENE

被引:24
作者
HUGHES, RP [1 ]
KOWALSKI, AS [1 ]
LOMPREY, JR [1 ]
RHEINGOLD, AL [1 ]
机构
[1] UNIV DELAWARE,DEPT CHEM,NEWARK,DE 19716
关键词
D O I
10.1021/om00019a027
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
The titanium promoted cyclization of the diketone ButC(O)CH2CH2CH2C(O)Bu(t), 1, affords 1,2-di-tert-butyl-1,2-cyclopentanediol, 2. Further reaction of 2 with POCl3 in hot pyridine results in dehydration to give the new vicinally di-tert-butyl-substituted cyclopentadiene, 3, which exists mainly as the 1,5-di-tert-butylcyclopentadiene tautomer 3b. As with other cyclopentadienes, 3 reacts cleanly with Bu(n)Li to give the corresponding lithium cyclopentadienide, 4, which in turn reacts with FeCl2.2THF to form 1,1',2,2'-tetra-tert-butylferrocene, 5. The structure of 5 has been confirmed by single crystal X-ray crystallography: Crystal data for 5 with Mo Kalpha (lambda = 0.7107 angstrom) radiation at 246 K: C26H42Fe, a = 16.135(3) angstrom, b = 8.416(1) angstrom, c = 16.800(3) angstrom, orthorhombic space group Cmca (No. 64), Z = 4, R = 0.0543, R(w) = 0.0734.
引用
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页码:2691 / 2695
页数:5
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