Hexa-, hepta-, and octacyclic ladder polysilanes

Chemistry Letters

Volumn 35, Issue 2, 2006, Pages 182-183

  Kyushin, Soichiro ^a   Ueta, Yoshinori ^a   Tanaka, Ryoji ^a   Matsumoto, Hideyuki ^a  

^a GUNMA UNIVERSITY   (Japan)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 33646457280     PISSN: 03667022     EISSN: None     Source Type: Journal    
DOI: 10.1246/cl.2006.182     Document Type: Article

References (21)

1. For recent reviews on ladder polysilanes, see: a) H. Matsumoto, S. Kyushin, M. Unno, R. Tanaka, J. Organomet. Chem. 2000, 611, 52.
2. b) S. Kyushin, H. Matsumoto, Adv. Organomet. Chem. 2003, 49, 133.
3. a) H. Matsumoto, H. Miyamoto, N. Kojima, Y. Nagai, J. Chem. Soc., Chem. Commun. 1987, 1316.
4. b) H. Matsumoto, H. Miyamoto, N. Kojima, Y. Nagai, M. Goto, Chem. Lett. 1988, 629.
5. c) S. Kyushin, H. Yamaguchi, T. Okayasu, Y. Yagihashi, H. Matsumoto, M. Goto, Chem. Lett. 1994, 221.
6. d) S. Kyushin, M. Kawabata, Y. Yagihashi, H. Matsumoto, M. Goto, Chem. Lett. 1994, 997.
7. e) S. Kyushin, H. Sakurai, H. Yamaguchi, M. Goto, H. Matsumoto, Chem. Lett. 1995, 815.
8. f) S. Kyushin, H. Sakurai, H. Yamaguchi, H. Matsumoto, Chem. Lett. 1996, 331.
9. g) S. Kyushin, Y. Yagihashi, H. Matsumoto, J. Organomet. Chem. 1996, 521, 413.
10. h) S. Kyushin, R. Tanaka, K. Arai, A. Sakamoto, H. Matsumoto, Chem. Lett. 1999, 1297.
11. i) S. Kyushin, A. Meguro, M. Unno, H. Matsumoto, Chem. Lett. 2000, 494.
12. j) S. Kyushin, Y. Miyajima, H. Matsumoto, Chem. Lett. 2000, 1420.
13. k) A. Meguro, H. Sakurai, K. Kato, S. Kyushin, H. Matsumoto, Chem. Lett. 2001, 1212.
14. l) R. Tanaka, S. Kyushin, M. Unno, H. Matsumoto, Enantiomer 2002, 7, 157.
15. m) M. Unno, R. Tanaka, S. Tanaka, T. Takeuchi, S. Kyushin, H. Matsumoto, Organometallics 2005, 24, 765.
16. A solution of 1,1,4,4-tetrachloro-1,2,2,3,3,4-hexaisopropyl-tetrasilane (2.47 g, 4.82 mmol) and 1,1,2,2-tetrachloro-1,2-diisopropyldisilane (2.77 g, 9.75 mmol) in THF (30 mL) was added dropwise to a mixture of lithium (0.39 g, 56 mmol) and THF (90 mL) at room temperature. The reaction mixture was stirred at room temperature for 1 day. After the solvent was removed by evaporation, the residue was dissolved in hexane, and the mixture was filtered through a short column of silica gel. The filtrate was evaporated, and the residue was separated by recycle-type HPLC (ODS, methanol-THF (55:45)) to give 2 (32.2 mg, 1.2%), 3 (50.5 mg, 2.0%), 4 (63.9 mg, 2.6%), 5 (19.1 mg, 0.8%), 6 (8.1 mg, 0.3%) and 7 (3.9 mg, 0.2%).
17. -3, R1 = 0.066 (I > 2σ(I)), wR2 = 0.208 (all data).
18. -3, R1 = 0.089 (I > 2σ(I)), wR2 = 0.246 (all data).
19. -3, R1 = 0.045 (I > 2σ(I)), wR2 = 0.144 (all data).
20. Crystallographic data reported in this manuscript have been deposited with Cambridge Crystallographic Data Centre as supplementary publication nos. CCDC-290140 (5), CCDC-290139 (6), and CCDC-290138 (7). Copies of the data can be obtained free of charge via www.ccdc.cam.ac.uk/conts/retrieving.html (or from the Cambridge Crystallographic Data Centre, 12, Union Road, Cambridge, CB2 1EZ, UK; fax: +44 1223 336033; or deposit@ccdc.cam.ac.uk).
21. Molecular A and molecular B denote two independent molecules present in a unit cell of the crystal of 5.