반응 #1148660

반응 방정식

bis(triethoxysilyl)methane

BTM

t-butyllithium

→

[bis(triethoxysilyl)methyl]lithium

반응 조건

후처리

1. 1
   workup.DISTILLATIONTo 300 mL of freshly distilled dry tetrahydrofuran (THF) in a 3-neck flask
2. 2
   기타the solution was flushed for 5 minutes with nitrogen that
3. 3
   기타resulted
4. 4
   온도Then the temperature of the solution was raised to room temperature (RT)
5. 5
   workup.STIRRINGstirring
6. 6
   workup.WAITcontinued for 30 minutes at RT

실험 절차

A commercially available bis(triethoxysilyl)methane (BTM) was lithiated by the following procedure. To 300 mL of freshly distilled dry tetrahydrofuran (THF) in a 3-neck flask attached to a bubbler was added 3.07 g (9.00 mmol) BTM and the solution was flushed for 5 minutes with nitrogen that had been passed through a drying column packed with CaCl2 and Drierite. The solution was cooled down to −78° C. and then 5.2 mL, 1.7 M (9 mmol) of t-butyllithium was added dropwise over 10 minutes. The solution was stirred for 30 minutes at −78° C. after which a very, faint yellowish solution resulted. Then the temperature of the solution was raised to room temperature (RT) and stirring continued for 30 minutes at RT after which the solution turned colorless.

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