Methyltrimethoxysilane → HCID 86712059, compound

Participants

Reaction Steps

A 500 ml 5-neck round-bottom flask rendered inert with nitrogen and equipped with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser is charged with 20 g (0.085 mol) of isooctyltrimethoxysilane (=2,4,4-trimethyl-1-pentyltrimethoxysilane, available commercially from Wacker Chemie AG as SILRES® BS 1316), 35 g (0.25 mol) of methyltrimethoxysilane (available commercially from Wacker Chemie AG), and 41 g of Isopar E (isoparaffinic hydrocarbon mixture with a boiling range of 113-143° C., available commercially from ExxonMobil). With stirring at 300 rpm, 32.1 g of 50% strength potassium hydroxide solution (0.286 mol KOH) are metered in over 10 minutes. This is followed by heating to reflux, with the water separator filled to the brim with Isopar E. The distillate separates out as the lower phase in the water separator. Up to a boiling temperature of 118° C., 41.4 g of clear colorless distillate are collected, which according to analysis by gas chromatography contains 80.4% methanol and 18.4% water. The hydrolysis of the methoxy radicals, accordingly, is quantitative. During the distillation, the reaction mixture undergoes transformation into a suspension. The volatile constituents are removed by distillation at 100° C./4 hPa. The residue left is 46.3 g of a white, coarse powder whose solids content is 99.9% (determined using the HR73 Halogen Moisture Analyzer solids content balance from Mettler Toledo at 160° C.)

Provenance & Evidence