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HRID 1274508생성일: 2026년 10월 27일

Iodine → tert-Butyldiphenylchlorosilane

https://huagongshe.com/reaction/1274508

반응식

참여 물질

역할이름HCID투입량
반응물IodineHCID 807—
반응물DichlorodiphenylsilaneHCID 6627—
반응물tert-BUTYL CHLORIDEHCID 10486—
반응물MagnesiumHCID 5462224—
반응물HCID 178418310HCID 178418310—
촉매Copper, bis(2,4-pentanedionato-O,O')-, (SP-4-1)-HCID 5363992—
용매1,2-DimethoxyethaneHCID 8071—
생성물tert-ButyldiphenylchlorosilaneHCID 9407885%

반응 조건

온도70 °C

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

DOI10.6084/m9.figshare.5104873.v1
특허 번호US06156918
출처 데이터셋uspto-grants-2000_12
ORD IDord-cbde98aec9034104afcedb1ef2902e1d
출처 메모uspto-grants-2000_12