Preparation of titanocenes

Abstract

A method for producing dialkylsilylbis(2-alkyl-4-aryl indenyl) titanocenes including rac-Me 2 Sibis(2-methyl-4-phenylindenyl)-titanium dichloride is described.

1. A method for preparing a dialkylsilylbis(2-alkyl-4-arylindenyl) titanium dichloride which comprises:
 (i) reacting a 2-alkyl-4-arylindene with an alkali metal alkyl and a dihalodialkyl silane to provide a first reaction mixture in a first reaction vessel;  
 (ii) separately reacting in a second reaction vessel titanium tetrachloride with and a second alkali metal alkyl which may be the same as or different from said first alkali metal alkyl to provide a second reaction mixture containing titanium trichloride in said second reaction vessel ; 
 wherein said second first reaction mixture contains a ligand of said dialkylsilylbis(2-alkyl-4-arylindenyl) titanium dichloride in which titanium is present in a plus three oxidation state;  
 
 (iii) containing said first and second reaction mixtures in the presence of an oxidizing agent; 
 wherein a third reaction mixture containing a mixture of rac and meso forms of said dialkylsilylbis(2-alkyl-4-arylindenyl) titanium dichloride is produced.  
 
 
     
     
       2. The  claim 1  method further comprising
 (iv) separating said mixture of rac and meso forms of said dialkylsilyl (2-alkyl-4-arylindenyl) titanium dichloride from said third reaction mixture.  
 
     
     
       3. The  claim 2  process further comprising separating said mixture of rac and meso forms of said dialkylsilyl (2-alkyl-4-arylindenyl) titanium dichloride from said third reaction mixture; and
 (v) separating said rac from said meso form of said dialkylsilyl (2-alkyl-4-arylindenyl) titanium dichloride.  
 
     
     
       4. The  claim 1  method in which said 2-alkyl-4-arylindene reacted in step (i) is 2-methyl-4-phenyl indene or 2-methyl-4-naphthyl indene or 2-methyl-4-anthracenyl indene and said step (iii) third reaction mixture contains a mixture of rac and meso forms of 2-methyl-4-phenyl indene or 2-methyl-4-naphthyl indene or 2-methyl-4-anthracenyl indene. 
     
     
       5. The  claim 1  method wherein said 2-alkyl-4-arylindene reacted in step (i) is 2-methyl-4-phenyl indene wherein said first and second alkali metal alkyls are each n-butyl lithium and wherein said step (iii) oxidizing agent is cuprous chloride or chloroform. 
     
     
       6. Rac-Me 2 Si(2-methyl-4-phenylindenyl)-titanium dichloride.