Synthesis and Structure of the First [1]Boratitanocenophanes

✍ Scribed by Holger Braunschweig; Carsten von Koblinski; Ruimin Wang

• Publisher: John Wiley and Sons
• Year: 1999
• Tongue: English
• Weight: 157 KB
• Volume: 1999
• Category: Article
• ISSN: 1434-1948
• DOI: 10.1002/(sici)1099-0682(199901)1999:1<69::aid-ejic69>3.0.co;2-l

✦ Synopsis

This paper presents two methods for the synthesis of the first reaction of [(Me 3 Si) 2 NB(C 5 H 5 ) 2 ], prepared in situ, with Ti(NMe 2 ) 4 and converted into the chloro derivatives [1]boratitanocenophanes. The novel biscyclopentadienylborane [(Me 3 Si) 2 NB(C 5 H 5 ) 2 ], the dilithio salt Li 2 [(Me 3 Si) 2 -[(Me 2 N)ClTi{(C 5 H 4 ) 2 BN(SiMe 3 ) 2 }] (4) and [Cl 2 Ti{(C 5 H 4 ) 2 BN-(SiMe 3 ) 2 }] (2) by treatment with one or two equivalents of a NB(C 5 H 4 ) 2 ] (1) of which was characterized by multinuclear NMR methods, was prepared in situ, and served as starting suitable diaminochloroborane. All [1]boratitanocenophanes were characterized in solution by multinuclear NMR material for several [1]boratitanocenophanes. [Cl 2 Ti{(C 5 H 4 ) 2 -BN(SiMe 3 ) 2 }] (2) was obtained in high yield by a convenient spectroscopy, and in addition the structure of 2 in the crystalline state was determined by a single-crystal X-ray one-pot synthesis starting from 1 and [TiCl 3 (thf) 3 ], followed by oxidation with PbCl 2 . The highly reactive study.