Improved Synthesis of HOPh₂Si-SiPh₂OH and Crystal Structure Analyses of HOPh₂Si-SiPh₂OH and HOPh₂Si-SiPh₂-O-Ph₂Si-SiPh₂OH·1/2C₆H₆

Abstract

1,1,2,2-Tetraphenyldisilane-1,2-diol (3) was prepared in a two-step synthesis, starting from 1,2-bis(diethylamino)-1,1,2,2-tetraphenyldisilane (1). Treatment of 1 with acetyl chloride yielded 1,2-dichloro-1,1,2,2-tetraphenyldisilane (2), which upon hydrolysis gave 3 (total yield 83%). Compounds 2 and 3 were characterized by elemental analyses (C,H) and solution NMR experiments (1H, 13C, 29Si; CDCl3). In addition, compound 1 and its condensation product, 1,5-dihydroxy-1,1,2,2,4,4,5,5-octaphenyl-3-oxa-1,2,4,5-tetrasilapentane (4; studied as the hemibenzene solvate 4ּ1/2C6H6), were structurally characterized by single-crystal X-ray diffraction.

(Me3N)Mo(CO)5-Catalyzed Reduction of DMF by Disiloxane and Disilane Moieties: Fate of the Silicon-Containing Fragments

“…The Si–Si bond length in 9c (2.376(2) Å; Table ) is statistically longer than the others due to the bulky Ph 3 Si substituents, and for example, in the other acyclic , the Si–Si bond distance is shorter because one of the Ph groups of 9c is replaced by a smaller hydroxyl group. The relationships between smaller SiOSi angles and longer Si–O bonds is maintained in this set of molecules . The presence of the hydroxyl groups also has a significant impact upon the Si–Si···Si–Si torsional angle for due to an intramolecular H bond between the two groups, as can be seen in Figures and and Table .…”

“…The relationships between smaller SiOSi angles and longer Si−O bonds is maintained in this set of molecules. 24 The presence of the hydroxyl groups also has a significant impact upon the Si−Si•••Si−Si torsional angle for OFUPIO due to an intramolecular H bond between the two groups, as can be seen in Figures 8 and 9 and Table 1. For the two cyclic molecules the torsional angle is ∼5°, for OFUPIO it averages ∼60°, and for 9c it is ∼151°.…”

Synthesis and Characterization of a Variety of α,ω-Bisacylpolysilanes─A Study on Reactivity and Accessibility

“…Recrystallization from n -heptane at −30 °C gave the product in 89% yield (30.0 g) as a white solid. The analytical data is identical to the reported data …”

Synthesis and Properties of Branched Hydrogenated Nonasilanes and Decasilanes

“…1 H (299.95 MHz) and 29 Si (59.59 MHz) NMR spectra were recorded on a Varian INOVA 300 spectrometer and referenced versus TMS using the internal 2 H-lock signal of the solvent or of internal D 2 O capillaries. Compounds 1 , 6 , and Cl­(SiPh 2 ) 2 Cl ,, were synthesized according to published procedures. Mass spectra were run on an HP 5971/A/5890-II GC/MS coupling (HP 1 capillary column, length 25 m, diameter 0.2 mm, 0.33 μm poly­(dimethylsiloxane)) or on a Kratos Profile mass spectrometer equipped with a solid probe inlet (HRMS).…”