تفاعل #1148660

ord-56ec9beedeac474d9ecb0826c96b1080

معادلة التفاعل

CCO[Si](C[Si](OCC)(OCC)OCC)(OCC)OCC
bis(triethoxysilyl)methane
CCO[Si](C[Si](OCC)(OCC)OCC)(OCC)OCC
BTM
[Li][C](C)(C)C
t-butyllithium
[Li][CH]([Si](OCC)(OCC)OCC)[Si](OCC)(OCC)OCC
[bis(triethoxysilyl)methyl]lithium

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
-78°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.DISTILLATIONTo 300 mL of freshly distilled dry tetrahydrofuran (THF) in a 3-neck flask
  2. 2
    أخرىthe solution was flushed for 5 minutes with nitrogen that
  3. 3
    أخرىresulted
  4. 4
    درجة الحرارةThen the temperature of the solution was raised to room temperature (RT)
  5. 5
    workup.STIRRINGstirring
  6. 6
    workup.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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06960551B2uspto-grants-2005_11