反应详情

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 60 g (0.44 mol) of methyltrimethoxysilane (available commercially from Wacker Chemie AG), and 100 g of 25% strength potassium hydroxide solution (0.44 mol KOH) are metered in over 10 minutes at 68° C. Following distillative removal of the methanol that is liberated, a clear, colorless solution is obtained. It is admixed with 77.2 g of Isopar E (isoparaffinic hydrocarbon mixture with a boiling range of 113-143° C., available commercially from ExxonMobil) and heated to reflux. The distillate separates out in the water separator as the lower phase, and at the same time a finely particulate suspension is formed in the reaction flask. As soon as water no longer separates out, the residue is evaporated to dryness at 100° C./4 hPa. 46.3 g of a white, fine powder are isolated, with a solids content of 99.8% (determined using the HR73 Halogen Moisture Analyzer solids content balance from Mettler Toledo at 160° C.).

1. customA 500 ml 5-neck round-bottom flask rendered inert with nitrogen
2. customequipped with paddle stirrer
3. temperaturewith reflux condenser
4. customare metered in over 10 minutes at 68° C
5. customremoval of the methanol that
6. customa clear, colorless solution is obtained
7. temperatureavailable commercially from ExxonMobil) and heated to reflux
8. customat the same time a finely particulate suspension is formed in the reaction flask
9. customthe residue is evaporated to dryness at 100° C./4 hPa
10. custom46.3 g of a white, fine powder are isolated, with a solids content of 99.8% (
11. customat 160° C.