Reaktion #2467085

ord-d4d30c271a5a413ab29ed7fb832db57c

Reaktionsgleichung

Cl[Si](Cl)(c1ccccc1)c1ccccc1
diphenyldichlorosilane
C[Si](C)(C)O
trimethylsilanol
CCN(CC)CC
triethylamine
C[Si](C)(C)O[Si](Cl)(c1ccccc1)c1ccccc1
trimethylsiloxydiphenylchlorosilane
Ausbeute 71.4%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwere introduced into a stirrer-equipped four-neck flask
  2. 2
    workup.ADDITIONwas added dropwise
  3. 3
    workup.WAITwas continued for an additional hour
  4. 4
    workup.ADDITIONcompletion of the addition
  5. 5
    Sonstigeat which time the salt formed as a by-product of the reaction
  6. 6
    Sonstigewas removed by filtration
  7. 7
    workup.DISTILLATIONThe filtrate was then distilled under reduced pressure

Vorschrift

The following were ingredients were introduced into a stirrer-equipped four-neck flask: 164.8 g (651.2 mmol) diphenyldichlorosilane and 300 mL tetrahydrofuran. The resultant mixture was stirred at room temperature while a mixture of 60 g (542.7 mmol) of 81.4% pure trimethylsilanol and 65.9 g (651.2 mmol) of triethylamine was added dropwise. Stirring at room temperature was continued for an additional hour following completion of the addition, at which time the salt formed as a by-product of the reaction was removed by filtration. The filtrate was then distilled under reduced pressure to yield 118.7 g of a fraction boiling at 136.5° C.-142° C. under of 2 mm Hg, equivalent to a 71.4% yield of trimethylsiloxydiphenylchlorosilane. Analysis of this product by gas chromatography (GLC), nuclear magnetic resonance (NMR), and infrared spectrochemical analysis (IR) confirmed it to be trimethylsiloxydiphenylchlorosilane with the following structural formula. ##STR6##

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05364896uspto-grants-1994_11