The Syntheses and Characterization of the Bulky Terphenyl Silanes and Chlorosilanes 2,6-Mes₂C₆H₃SiCl₃, 2,6-Trip₂C₆H₃SiCl₃, 2,6-Mes₂C₆H₃SiHCl₂, 2,6-Trip₂C₆H₃SiHCl₂, 2,6-Mes₂C₆H₃SiH₃, 2,6-Trip₂C₆H₃SiH₃ and 2,6-Mes₂C₆H₃SiC1₂SiC1₃

Article type: Research Article

Authors: Simons, Richard S. | Haubrich, Scott T. | Mork, Benjamin V. | Niemeyer, Mark | Power, Philip P.

Affiliations: Contribution from the Department of Chemistry, University of California, Davis, California 95616

Note: [] Corresponding author.

Abstract: The synthesis and characterization of the primary terphenyl silanes and chlorosilanes 2,6-Mes2C6H3SiCl3 (la), 2,6-Trip2C6H3SiHC3 (lb), 2,6-Mes2C6H3SiHCl2 (2a), 2,6-Trip2C6H3. SiHC12 (2b), 2,6-Mes2C6H3SiH3 (3a), 2,6-Trip2C6SiH3 (3b) and 2,6-Mes2C6H3siCl2-SiCl3 (4), (where Mes = 2,4,6-Me3C6H2 and Trip = 2,4,6-i-Pr3C6H2) are described. Compounds (la, lb), (2a, 2b) and (4) were prepared by the reaction between SiC14, SiHCl3 or Si2C16, respectively, and the appropriate aryl lithium reagent (2,6-Mes2C6H3Li or 2,6-Trip2C6H3Li·OEt2). Compounds (3a) and (3b) were prepared by reduction of (1a) and (1b) with LiA1H4, respectively. The derivatives (la) – (3a) were characterized by 1H, 13C, 29Si NMR and IR spectroscopy. The structures of (la), (lb) and (4) have been determined. Crystal data with Cu Kα (λ = 1.54178 Å) at 130 K: (la), a = 9.074(2) Å, b = 16.681(3) Å, c = 15.842 (3) Å, β = 105.20(3)°, V = 2313.9(8) Å3, Z = 4, space group P21/c, 2772 (I > 2σ(I)) data, R = 0.042; (lb), a = 12.197(2) Å, b = 25.602(5) Å, c = 11.098(2) Å, V = 3465.5(11) Å3, Z = 4, space group Pnma, 2131 (I > 2σ(I)) data, R = 0.061; (4), a = 10.799(2) Å, b = 15.355(3) Å, c = 16.724(3) Å, β = 106.907(13)°, V = 2653.2(8) Å3, Z = 4, space group P21/n, 2852 (I > 2σ(I)) data, R = 0.047.

DOI: 10.1080/10241229812331341469

Journal: Main Group Chemistry, vol. 2, no. 4, pp. 275-283, 1998