Reaktion #2467085
ord-d4d30c271a5a413ab29ed7fb832db57c
Reaktionsgleichung
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1workup.ADDITIONwere introduced into a stirrer-equipped four-neck flask
- 2workup.ADDITIONwas added dropwise
- 3workup.WAITwas continued for an additional hour
- 4workup.ADDITIONcompletion of the addition
- 5Sonstigeat which time the salt formed as a by-product of the reaction
- 6Sonstigewas removed by filtration
- 7workup.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##