참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | Dichlorodiphenylsilane | HCID 6627 | — |
| 반응물 | tert-BUTYL CHLORIDE | HCID 10486 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 반응물 | HCID 178418310 | HCID 178418310 | — |
| 촉매 | Copper, bis(2,4-pentanedionato-O,O')-, (SP-4-1)- | HCID 5363992 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | tert-Butyldiphenylchlorosilane | HCID 94078 | 85% |
반응 단계
48.6 g (2.0 mol) of magnesium filings and a spatula-tip of iodine are initially introduced into a 2 1 three-necked flask with a precision glass stirrer, straight enclosed-scale thermometer, Dimroth condenser and dropping funnel under a blanket of inert gas. By addition of 600 ml of ethylene glycol dimethyl ether and 203.7 g (2.2 mol) of tert-butyl chloride, tert-butylmagnesium chloride is prepared. Initially 5.2 g (0.02 mol) of copper(II) acetylacetonate and then, at 50° C. over 2 hours, 455.8 g (1.8 mol) of diphenyldichlorosilane are subsequently added dropwise. The internal temperature of the flask rises slightly, and the mixture is subsequently stirred at 70° C. for a further 3 hours to bring the reaction to completion. To remove the precipitated magnesium salt from the solution, the reaction mixture is filtered through a pressure suction filter maintained under an argon atmosphere. The filter cake is rinsed with ethylene glycol dimethyl ether. A concluding fractional distillation of the combined filtrates in vacuo gives 420.6 g of tert-butyldiphenylchlorosilane (85% yield, based on the diphenyldichlorosilane) as a colorless liquid in a GC purity of 92%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06156918 |
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| 출처 데이터셋 | uspto-grants-2000_12 |
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| ORD ID | ord-cbde98aec9034104afcedb1ef2902e1d |
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| 출처 메모 | uspto-grants-2000_12 |
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