Phenyltris(dimethylsiloxy)silane synthesis
- Product Name:Phenyltris(dimethylsiloxy)silane
- CAS Number:18027-45-7
- Molecular formula:C12H26O3Si4
- Molecular Weight:330.67
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18027-45-7
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Yield:-
Reaction Conditions:
with hydrogenchloride in water;toluene at 47; for 1 h;Inert atmosphere;
Steps:
3
Example 3Preparation of the Precursor TPhMH3 2,010 g tetramethyldisiloxane (30 mol), 1,200 g water, 60 g 37% hydrochloric acid and 1,000 g toluene are received in a 61 flat flange vessel with a heating/cooling jacket equipped with a stirrer, thermometer, reflux condenser, dosing device and nitrogen blanketing. 1,586 g phenyltrimethoxysilane (8 mol) are metered in with vigorous stirring. Due to the reaction, the reaction mixture heats up to 47° C. during metering.After the metering process is completed, this is followed by stirring for one hour; after the stirrer has been switched off, 2 phases form rapidly. The lower aqueous phase is separated and discarded. The top organic phase is washed with 100 ml water. After the aqueous phase has been removed, the excess tetramethyldisiloxane is separated in a fractioned manner by distillation. The distillation process is stopped as soon as an overhead temperature of 110° C. has been reached.Analysis of the remaining bottom by gas chromatography yielded a composition of 45% by wt. TPhMH4, 21% TPh2MH6, 7.5% TPh3MH8 and 26.5% toluene (SiH content 6.2 mmol/g) and is added without further purification to the subsequent reaction of Example 4.
References:
US2012/46485,2012,A1 Location in patent:Page/Page column 5
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18027-45-7
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