反应详情

A slurry 89.3 g of Li metal cut into small pieces in 1500 ml dry tetrahydrofuran (THF) under an Ar atmosphere was treated dropwise with neat Ph2MeSiCl (1302.2g, 5.59 moles). During the addition, agitation was provided via a mechanical stirrer and an ice bath was employed as necessary to hold the reaction temperature under 40° C. The mixture was then allowed to stir overnight (16 hr.) at room temperature. The dark red solution of Ph2MeSiLi was then treated with 607.7g (5.59 moles) of Me3SiCl dissolved in 700 ml dry THF. Again an ice bath was utilized to maintain the reaction mixture temperature under 40° C. Near the end of the Me3SiCl addition, the red color of Ph2MeSiLi was completely discharged. Upon completion of the addition, the now essentially colorless mixture was filtered to remove precipitated LiCl and unreacted Li metal. Solvent was removed from the resulting clear solution at reduced pressure and the residual oil fractionally distilled at 0.3 mm Hg to afford 1074.1 g of title compound (71%), bp 108°-110° C.

1. additionDuring the addition
2. customagitation was provided via a mechanical stirrer and an ice bath
3. customunder 40° C
4. temperatureto maintain the reaction mixture temperature under 40° C
5. additionUpon completion of the addition
6. filtrationthe now essentially colorless mixture was filtered
7. customto remove
8. customprecipitated LiCl and unreacted Li metal
9. customSolvent was removed from the resulting clear solution at reduced pressure
10. distillationthe residual oil fractionally distilled at 0.3 mm Hg