tert-butyl(trichloro)silane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under argon, a reaction vessel fitted with a stirrer was charged with 100 ml diethylether and 11.7 g. t-butyltrichlorosilane (0.0615 mol) and stirring was commenced. To this vessel was added dropwise 6.34 g 1-lithio-4-methylpiperidine in diethylether solution from (b) above via a cannula over a 30 min. period and stirring was continued for about 16 hours. The vessel was fitted with a condenser and the reaction mixture was refluxed for 1 hr. and cooled to room temperature. The solution was filtered through a medium porosity frit and the LiCl precipitate was washed three times with 20 ml portions of diethylether. The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil. The crude product was distilled under vacuum (60°-68° C., @ 0.7 torr) to give a clear to slightly cloudy oil of 6.45 g of t-butyl(4methylpiperidyl)dichlorosilane. Under argon, a reaction vessel fitted with a stirrer The vessel was fitted with a condenser the reaction mixture was refluxed for 1 hr The solution was filtered through a medium porosity frit the LiCl precipitate was washed three times with 20 ml portions of diethylether The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil The crude product was distilled under vacuum (60°-68° C., @ 0.7 torr)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under argon, a reaction vessel fitted with a stirrer was charged with 100 ml diethylether and 11.7 g. t-butyltrichlorosilane (0.0615 mol) and stirring was commenced. To this vessel was added dropwise 6.34 g 1-lithio-4-methylpiperidine in diethylether solution from (b) above via a cannula over a 30 min. period and stirring was continued for about 16 hours. The vessel was fitted with a condenser and the reaction mixture was refluxed for 1 hr. and cooled to room temperature. The solution was filtered through a medium porosity frit and the LiCl precipitate was washed three times with 20 ml portions of diethylether. The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil. The crude product was distilled under vacuum (60°-68° C., @ 0.7 torr) to give a clear to slightly cloudy oil of 6.45 g of t-butyl(4methylpiperidyl)dichlorosilane. Under argon, a reaction vessel fitted with a stirrer The vessel was fitted with a condenser the reaction mixture was refluxed for 1 hr The solution was filtered through a medium porosity frit the LiCl precipitate was washed three times with 20 ml portions of diethylether The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil The crude product was distilled under vacuum (60°-68° C., @ 0.7 torr)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under argon, a reaction vessel fitted with a stirrer was charged with 100 ml diethylether and 11.7 g. t-butyltrichlorosilane (0.0615 mol) and stirring was commenced. To this vessel was added dropwise 6.34 g 1-lithio-4-methylpiperidine in diethylether solution from (b) above via a cannula over a 30 min. period and stirring was continued for about 16 hours. The vessel was fitted with a condenser and the reaction mixture was refluxed for 1 hr. and cooled to room temperature. The solution was filtered through a medium porosity frit and the LiCl precipitate was washed three times with 20 ml portions of diethylether. The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil. The crude product was distilled under vacuum (60°-68° C., @ 0.7 torr) to give a clear to slightly cloudy oil of 6.45 g of t-butyl(4methylpiperidyl)dichlorosilane. Under argon, a reaction vessel fitted with a stirrer The vessel was fitted with a condenser the reaction mixture was refluxed for 1 hr The solution was filtered through a medium porosity frit the LiCl precipitate was washed three times with 20 ml portions of diethylether The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil The crude product was distilled under vacuum (60°-68° C., @ 0.7 torr)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under argon, a reaction vessel fitted with a stirrer was charged with 100 ml diethylether and 11.7 g. t-butyltrichlorosilane (0.0615 mol) and stirring was commenced. To this vessel was added dropwise 6.34 g 1-lithio-4-methylpiperidine in diethylether solution from (b) above via a cannula over a 30 min. period and stirring was continued for about 16 hours. The vessel was fitted with a condenser and the reaction mixture was refluxed for 1 hr. and cooled to room temperature. The solution was filtered through a medium porosity frit and the LiCl precipitate was washed three times with 20 ml portions of diethylether. The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil. The crude product was distilled under vacuum (60-68° C., @0.7 torr) to give a clear to slightly cloudy oil of 6.45 g of t-butyl(4-methylpiperidyl)dichlorosilane. Under argon, a reaction vessel fitted with a stirrer The vessel was fitted with a condenser the reaction mixture was refluxed for 1 hr The solution was filtered through a medium porosity frit the LiCl precipitate was washed three times with 20 ml portions of diethylether The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil The crude product was distilled under vacuum (60-68° C., @0.7 torr)

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under argon, a reaction vessel fitted with a stirrer was charged with 100 ml diethylether and 11.7 g. t-butyltrichlorosilane (0.0615 mol) and stirring was commenced. To this vessel was added dropwise 6.34 g 1-lithio-4-methylpiperidine in diethylether solution from (b) above via a cannula over a 30 min. period and stirring was continued for about 16 hours. The vessel was fitted with a condenser and the reaction mixture was refluxed for 1 hr. and cooled to room temperature. The solution was filtered through a medium porosity frit and the LiCl precipitate was washed three times with 20 ml portions of diethylether. The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil. The crude product was distilled under vacuum (60°-68° C., @ 0.7 torr) to give a clear to slightly cloudy oil of 6.45 g of t-butyl(4methylpiperidyl)dichlorosilane. Under argon, a reaction vessel fitted with a stirrer The vessel was fitted with a condenser the reaction mixture was refluxed for 1 hr The solution was filtered through a medium porosity frit the LiCl precipitate was washed three times with 20 ml portions of diethylether The diethylether was removed from the filtrate in vacuo to provide a clear yellow oil The crude product was distilled under vacuum (60°-68° C., @ 0.7 torr)