Tetrakis Trimethylsilyl Silane Research Articles

ChemInform Abstract: Tetrakis(trimethylsilyl)silane-Mediated Photochemical Alkylation of Heteroaromatic Bases with Alkyl Halides.

Alkyl halides reacted with protonated heteroaromatic bases in the presence of tetrakis(trimethylsilyl)silane (TTMS) under irradiation with high pressure mercury lamp to give the corresponding alkylated heteroaromatic bases. This is the first report on the photochemical use of TTMS for organic synthesis.

Sensitivity considerations in polarization transfer and filtering using dipole–dipole couplings: Implications for biomineral systems

The robustness and sensitivities of different polarization-transfer methods that exploit heteronuclear dipole–dipole couplings are compared for a series of heterogeneous solid systems, including polycrystalline tetrakis(trimethylsilyl)silane (TKS), adamantane, a physical mixture of doubly 13C, 15N-enriched and singly 13C-enriched polycrystalline glycine, and a powder sample of siliceous marine diatoms, Thalossiosira pseudonana. The methods were analyzed according to their respective frequency-matching spectra or resultant signal intensities. For a series of 13C{ 1H} cross-polarization experiments, adiabatic passage Hartmann–Hahn cross-polarization (APHH-CP) was shown to have several advantages over other methods, including Hartmann–Hahn cross-polarization (HHCP), variable-amplitude cross-polarization (VACP), and ramped-amplitude cross-polarization (RACP). For X–Y systems, such as 13C{ 15N}, high and comparable sensitivities were obtained by using APHH-CP with Lee–Goldburg decoupling or by using the transferred-echo double resonance (TEDOR) experiment. The findings were applied to multinuclear 1H, 13C, 15N, and 29Si CP MAS characterization of a powder diatom sample, a challenging inorganic–organic hybrid solid that places high demands on NMR signal sensitivity.

High-resolution solid-state 13C and 29Si NMR investigations of the dynamic properties of tetrakis(trimethylsilyl)silane

High-resolution solid-state 13C and 29Si NMR spectroscopy have been used to investigate the dynamic properties of tetrakis(trimethylsilyl)silane (TTMSS) as a function of temperature; from the temperature dependence of the spectra, it is clear that TTMSS is not useful as a chemical shift reference material below ca. 238K, but the spectral changes associated with the phase transition at this temperature nevertheless provide a precise method for controlling temperature calibration in low-temperature solid-state 13C NMR studies.

Natural Abundance Solid State 2H NMR Studies of Phase Transitions in Rotator Phase Solids

Variable temperature natural abundance 2 H NMR studies of solid state phase transitions in adamantane, tetrakis(trimethylsilyl)methane (TTMSM), tetrakis(trimethylsilyl)silane (TTMSS) and 2,2-dimethyl-1,3-propanediol (DMPD) are reported; in spite of the low sensitivity associated with natural abundance 2 H NMR, this technique is demonstrated as a feasible approach for elucidating changes in molecular dynamic properties associated with the phase transitions in these materials.

Tetiakis(trimethylsilyl)silane-Mediated Photochemical Alkylation of Heteroaromatic Bases with Alkyl Halides

Abstract Alkyl halides reacted with protonated heteroaromatic bases in the presence of tetrakis(trimethylsilyl)silane (TTMS) under irradiation with high pressure mercury lamp to give the corresponding alkylated heteroaromatic bases. This is the first report on the photochemical use of TTMS for organic synthesis.