BIS(TRIETHOXYSILYL)METHANE → HCID 178506912, Verbindung

HRID 1061478Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1061478
[CH2:1]([O:3][Si:4]([CH2:11][Si:12]([O:19][CH2:20][CH3:21])([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15])([O:8][CH2:9][CH3:10])[O:5][CH2:6][CH3:7])[CH3:2].C([Li:26])(C)(C)C>>[CH2:17]([O:16][Si:12]([CH:11]([Li:26])[Si:4]([O:8][CH2:9][CH3:10])([O:5][CH2:6][CH3:7])[O:3][CH2:1][CH3:2])([O:19][CH2:20][CH3:21])[O:13][CH2:14][CH3:15])[CH3:18]

Komponenten

3

Edukt 2

HCID 9798044BIS(TRIETHOXYSILYL)METHANE2×HCID 178418306HCID 178418306, Verbindung

Produkt 1

HCID 178506912HCID 178506912, Verbindung

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

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.

Aufarbeitung

  1. distillationTo 300 mL of freshly distilled dry tetrahydrofuran (THF) in a 3-neck flask
  2. customthe solution was flushed for 5 minutes with nitrogen that
  3. customresulted
  4. temperatureThen the temperature of the solution was raised to room temperature (RT)
  5. stirringstirring
  6. waitcontinued for 30 minutes at RT

Quellen und Nachweise

ORD-Eintrag
ord-56ec9beedeac474d9ecb0826c96b1080
Quelldatensatz
uspto-grants-2005_11
Patentnummer
US06960551B2

Notizen zur Reaktion

Wird geladen…