Reaktion #65875

Reaktionsgleichung

hexamethyldisilazane

lithium

hydrogen

→

lithium hexamethyldisilazane

Ausbeute 90.0%

Lösungsmittel

hexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was then cooled to below 40° C.
2. 2
   workup.DISSOLUTIONto dissolve the product
3. 3
   FiltrationFiltration
4. 4
   Sonstigeto remove any unreacted lithium metal
5. 5
   Sonstigefollowed by evaporation under vacuum (2 mm Hg) at 110° C.

Vorschrift

To 288 ml of hexamethyldisilazane (220 g, 1.36 mole) in a 1-liter Parr reactor was charged 7.00 g of lithium metal (1.00 mole) under an argon atmosphere, with a backpressure of approximately 150 psig. The mixture was slowly heated to 225° C. over a 1 to 2 hour period. At this temperature and pressure, the reaction was allowed to proceed for approximately 16 hours with stirring and venting of hydrogen. The reaction mixture was then cooled to below 40° C. and hexane solvent (300 ml) was added to dissolve the product. Filtration to remove any unreacted lithium metal followed by evaporation under vacuum (2 mm Hg) at 110° C. provided approximately 150 g of lithium hexamethyldisilazane solid (approximately 0.90 mole, >90% yield, total base analysis: 101.3% of the theoretical value).

Quelle