関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichlorodiphenylsilane | HCID 6627 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Trimethylsilanol | HCID 66110 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Trimethylsiloxydiphenylchlorosilane | HCID 19417892 | 71.4% |
反応手順
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##
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05364896 |
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| 出典データセット | uspto-grants-1994_11 |
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| ORD ID | ord-d4d30c271a5a413ab29ed7fb832db57c |
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| 出典メモ | uspto-grants-1994_11 |
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