Novel Synthesis of Unbridged, Sterically Substituted Zirconocene Dichlorides from Fulvenes and Dialkylzirconium Dichlorides via Zirconium(IV) Hydride Transfer

Organometallics

Volumn 18, Issue 9, 1999, Pages 1583-1585

  Eisch, John J ^a   Owuor, Fredrick A ^a   Shi, Xian ^a  

^a BINGHAMTON UNIVERSITY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0000003352     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om981048c     Document Type: Article

References (20)

1. Part 17 of the series Organic Chemistry of Subvalent Transition Metal Complexes. Part 16: Eisch, J. J.; Shi, X.; Owuor, F. A. Organometallics 1998, 17, 5219.
2. Eisch, J. J.; Shi, X.; Owuor, F. A. Organometallics 1998, 17, 5219.
3. 2 confirm that it is indeed the racemic isomer (personal communication from Professor A. L. Rheingold, University of Delaware).
4. 2 and thereby leave as open questions both the state of actual aggregation of such units and the possible role of ate-complexation of the LiCl.
5. 2ZrHCl, had of course been established almost 25 years ago: Hart, D. W.; Schwartz, J. J. Am. Chem. Soc. 1974, 96, 8115. Hart, D. W., Blackburn, T. F.; Schwartz, J. J. Am. Chem. Soc. 1976, 97, 679.
6. 2ZrHCl, had of course been established almost 25 years ago: Hart, D. W.; Schwartz, J. J. Am. Chem. Soc. 1974, 96, 8115. Hart, D. W., Blackburn, T. F.; Schwartz, J. J. Am. Chem. Soc. 1976, 97, 679.
7. (a) Eisch, J. J.; Shi, X.; Alila, J. R.; Thiele, S. Chem. Ber. /Rec. 1997, 130, 1175.
8. (b) Shi, X. Doctoral Dissertation, State University of New York at Binghamton, May, 1996.
9. 2 angle is drawn down to 75.4°. Although the putative agostic β-H is not observed directly, the angle contraction from 109° to 75° supports the operation of such an interaction: Kaminsky, W.; Kopf, Jürgen; Sinn, H.; Vollmer, H.-J. Angew. Chem., Int. Ed. Engl. 1976, 15, 629.
10. Eisch, J. J.; Boleslawski, M. P. J. Organomet. Chem. 1987, 334, C1.
11. All operations and reactions were carried out under an atmosphere of anhydrous, deoxygenated argon, and solvents and reaction vessels were likewise dried and deoxygenated before use. For relevant techniques: Eisch, J. J. Organometallic Syntheses; Academic Press: New York, 1981; Vol. 2, pp 3-62.
12. 2).
13. Eisch, J. J.; Shi, X.; Lasota, J. Z. Naturforsch. 1995, 50b, 342.
14. 13C NMR δ 142.04, 114.63, 111.99, 28.74, 23.15.
15. 13C NMR δ 142.1, 129.8, 128.3, 127.9, 118.79, 113.59, 108.32.
16. 2.
17. 2CH-OH(D), undeuterated on the benzylic carbon.
18. (a) The test polymerizations of ethylene were carried out in the manner described in ref 2.
19. 2-symmetry axis, as that possessed by bis(tert-butylcyclopentadienyl)zirconium dichloride and its many derivatives (cf. 20): (Erker, G.; Muhlenberd, T.; Nolte, R.; Peterson, J. L.; Tainturier, G.; Gautheron, B. J. Organomet. Chem. 1986, 314, C21. Krüger, C.; Nolte, M.; Erker, G.; Thiele, S. Z. Naturforsch. 1992, 47b, 995.
20. 2-symmetry axis, as that possessed by bis(tert-butylcyclopentadienyl)zirconium dichloride and its many derivatives (cf. 20): (Erker, G.; Muhlenberd, T.; Nolte, R.; Peterson, J. L.; Tainturier, G.; Gautheron, B. J. Organomet. Chem. 1986, 314, C21. Krüger, C.; Nolte, M.; Erker, G.; Thiele, S. Z. Naturforsch. 1992, 47b, 995.