Cyclohexasiloxane synthesis

Yield:295-01-2 57.6%

Reaction Conditions:

in hexane;Cooling;

Steps:

5

A Schlenk vessel (100 ml) with a magnetic stirrer bar is initially charged with 2.51 g (20 mmol) of zinc carbonate in 40 ml of n-hexane with ice cooling. Through a septum, with a syringe, 4.23 ml (20 mmol of dichlorosilane) of a 40% mixture of n-hexane and dichlorosilane are added. After the evolution of gas has ended, the solid is filtered off from the solution through a Schlenk frit, and the solvent is removed by means of a low temperature distillation (generation of vacuum with liquid nitrogen, room temperature and pressure less than 100 hPa). After 5 min, new n-hexane was added, followed by characterization by means of NMR spectroscopy, as described in working example 1 (yield 57.6%).²⁹Si NMR Spectrum:δ(H₂SiO)₆=-48.8 ppm ¹H NMR Spectrum: δ(H₂SiO)₆=approx. 4.7 ppm The NMR data show that the desired compound (H₂SiO)₆ is present in a purity of greater than 95%.

References:

US7655206,2010,B2 Location in patent:Page/Page column 7