Chlorotrimethylsilane → (Diethylamino)trimethylsilane

Temperature

55 °C

In a 1 liter four-neck flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer were placed 108.5 g (1.0 mol) of trimethylchlorosilane, 111.1 g (1.1 mol) of triethylamine and 300 ml of hexane. Thereto, 73.0 g (1.0 mol) of diethylamine was added dropwise from the dropping funnel over a 1-hour period. During the addition, the temperature of the reaction system was kept within the range of 20° C. to 60° C. to make the reaction be proceeding. At the conclusion of the addition, the temperature was raised to 50-60° C. and kept there for 2 hours, whereby the reaction was matured. Then, the reaction mixture was filtered through a glass filter to remove the salt yielded as a by-product. The filtrate was allowed to stand for one day at room temperature to precipitate the salt. The salt precipitated was filtered off, and the filtrate was subjected to distillation under ordinary pressure to obtain 136.3 g of diethylaminotrimethylsilane as a fraction having a boiling point of 125-126° C. The yield was 94%, and the chlorine concentration was 146 ppm.

1. customIn a 1 liter four-neck flask equipped with a stirrer, a reflux condenser, a dropping funnel
2. additionDuring the addition
3. customwas kept within the range of 20° C. to 60° C.
4. additionAt the conclusion of the addition
5. filtrationThen, the reaction mixture was filtered through a glass
6. filtrationfilter
7. customto remove the salt
8. customyielded as a by-product
9. waitto stand for one day at room temperature
10. customto precipitate the salt
11. customThe salt precipitated
12. filtrationwas filtered off
13. distillationthe filtrate was subjected to distillation under ordinary pressure

ORD record

ord-fbc2973383d04e348e7380fd91ee5de8

Source dataset

uspto-grants-1992_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05142080