Synthesis of novel titanasiloxanes with ring and cage structures using sterically demanding substituents

Nolte JO, Schneider M, Neumann B, Stammler H-G, Jutzi P (2003)
ORGANOMETALLICS 22(5): 1010-1017.

Journal Article | Published | English

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Abstract
Novel oligomeric titanasiloxanes have been synthesized in good yields by reaction of sterically demanding organosilanetriols with titanium alkoxides. The silanetriols Bu-t(2)(Me3Si)FlSi(OH)(3) (5), (Me3Si)FlSi(OH)(3) (6), and MeFlSi(OH)(3) (7) and the titanium alkoxides Ti((OEt)-Et-i)(4), Ti((OPr)-Pr-i)(4), and Ti((OPr)-Pr-i)(2)(acac)(2) have been used as starting materials (Fl = fluorenyl). Quite different structures are obtained by only small modifications of the organic substituents of the substrates. Thus, the condensation reactions result in the formation of the polyhedral titanasiloxanes [Bu-t(2)(Me3Si)FlSi](4)O-12[TiOEt](4) (8), [(Me3Si)FlSi](2)O-5[Ti(OEt)](4) /mu(2)-OEt](6) [mu(4)-O] (9), ([Bu-t(2)(Me3Si)FlSi](3)O-10[Ti((OPr)-Pr-i)](4) [mu(2)-OiPr](2) [mu(3)-O]Ti)(2)O (10), and [MeFlSi](2)O-8[Ti((OPr)-Pr-i)](6)(-) [mu(2)-(OPr)-Pr-i](4)[mu(3)-O](2)[PhNH2](2) (11) and the cyclic titanasiloxane [MeFlSi((OPr)-Pr-i)](2)O-4[Ti(acac)(2)](2) (12). A 1:1 stoichiometry of the starting materials leads to 8 and 12 in quantitative yield, while 9-11 are isolated in minor quantities. If the appropriate substrate ratio is used, the latter compounds can also be obtained in high yields. All titanasiloxanes have been characterized by X-ray crystallography, NMR, IR, and elemental analysis.
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Nolte JO, Schneider M, Neumann B, Stammler H-G, Jutzi P. Synthesis of novel titanasiloxanes with ring and cage structures using sterically demanding substituents. ORGANOMETALLICS. 2003;22(5):1010-1017.
Nolte, J. O., Schneider, M., Neumann, B., Stammler, H. - G., & Jutzi, P. (2003). Synthesis of novel titanasiloxanes with ring and cage structures using sterically demanding substituents. ORGANOMETALLICS, 22(5), 1010-1017.
Nolte, J. O., Schneider, M., Neumann, B., Stammler, H. - G., and Jutzi, P. (2003). Synthesis of novel titanasiloxanes with ring and cage structures using sterically demanding substituents. ORGANOMETALLICS 22, 1010-1017.
Nolte, J.O., et al., 2003. Synthesis of novel titanasiloxanes with ring and cage structures using sterically demanding substituents. ORGANOMETALLICS, 22(5), p 1010-1017.
J.O. Nolte, et al., “Synthesis of novel titanasiloxanes with ring and cage structures using sterically demanding substituents”, ORGANOMETALLICS, vol. 22, 2003, pp. 1010-1017.
Nolte, J.O., Schneider, M., Neumann, B., Stammler, H.-G., Jutzi, P.: Synthesis of novel titanasiloxanes with ring and cage structures using sterically demanding substituents. ORGANOMETALLICS. 22, 1010-1017 (2003).
Nolte, JO, Schneider, M, Neumann, B, Stammler, Hans-Georg, and Jutzi, Peter. “Synthesis of novel titanasiloxanes with ring and cage structures using sterically demanding substituents”. ORGANOMETALLICS 22.5 (2003): 1010-1017.
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