1,4-DISILABUTANE synthesis

Yield:4364-07-2 65%

Reaction Conditions:

with lithium aluminium tetrahydride in dibutyl ether at -78 - 25; for 2 h;Inert atmosphere;

Steps:

1 Syntheses of starting materials 1 ,2-disilapropane (DSP) and 1 ,3- disilabutane (DSB)

General procedure: Lithium aluminium hydride LiAIH₄(LAH) was placed into a 4L vessel equipped with a mechanical stirrer under inert atmosphere. The vessel was cooled to -78°C, and then 1 L of cold (ca. -30°C) diglyme (H₃COC₂H₄OC₂H₄OCH3) for DSP or di-nbutyl ether (H₉C₄OC₄H₉) for DSB was slowly added to the vessel. The mixture in the vessel was allowed to warm to -10°C while stirring. 1 ,2-bis(trichlorosilyl)methane SiCI₃CH₂SiCI₃or 1 ,2-bis(trichlorosilyl)ethane SiCI₃CH₂CH₂SiCI₃was added dropwise to the warmed mixture, while preventing the reaction mixture from getting warmer than 20°C. After the addition, the mixture was warmed to 25°C and stirred for 2 hours. The volatile DSP or DSB was condensed into a trap (-78°C) at 30°C. DSP was isolated in 82% yield, 96% purity shown by Gas Chromatography (GC). DSB was isolated as color less liquid. Yield 65%, 98.8% purity shown by GC.

References:

WO2016/160991,2016,A1 Location in patent:Paragraph 00117-00118