تفاعل #1148660
ord-56ec9beedeac474d9ecb0826c96b1080
معادلة التفاعل
الكواشف
ظروف التفاعل
المعالجة
- 1workup.DISTILLATIONTo 300 mL of freshly distilled dry tetrahydrofuran (THF) in a 3-neck flask
- 2أخرىthe solution was flushed for 5 minutes with nitrogen that
- 3أخرىresulted
- 4درجة الحرارةThen the temperature of the solution was raised to room temperature (RT)
- 5workup.STIRRINGstirring
- 6workup.WAITcontinued for 30 minutes at RT
الإجراء التجريبي
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.