反応 #65875

反応方程式

hexamethyldisilazane

lithium

hydrogen

→

lithium hexamethyldisilazane

収率 90.0%

溶媒

hexane

反応条件

後処理

1. 1
   温度The reaction mixture was then cooled to below 40° C.
2. 2
   workup.DISSOLUTIONto dissolve the product
3. 3
   ろ過Filtration
4. 4
   その他to remove any unreacted lithium metal
5. 5
   その他followed by evaporation under vacuum (2 mm Hg) at 110° C.

実験手順

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).

出典