참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Chlorotrimethylsilane | HCID 6397 | — |
| 반응물 | Chlorobenzene | HCID 7964 | — |
| 반응물 | Diphenyl sulfoxide | HCID 13679 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Triphenylsulfonium chloride | HCID 61343 | — |
반응 단계
Into 400 g of dichloromethane was dissolved 40 g (0.2 mole) of diphenyl sulfoxide, and the resulting solution was agitated under ice-cool. And then, 65 g (0.6 mole) of trimethyl silyl chloride was added dropwise at the temperature not exceeding 20° C., at which temperature the mixture was aged for 30 minutes. Thereafter, a Grignard agent prepared separately from 14.6 g (0.6 mole) of a metal magnesium, 67.5 g (0.6 mol) of chlorobenzene, and 168 g of tetrahydrofurane (THF) was added dropwise into it at the temperature not exceeding 20° C. After the reaction mixture was aged for one hour, it was added by 50 g of water at the temperature not exceeding 20° C. to terminate the reaction, and then further by 150 g of water, 10 g of 12-N hydrochloric acid, and 200 g of diethyl ether. A water layer was taken out by separation and washed by 100 g of diethyl ether to obtain an aqueous triphenyl sulfonium chloride solution. This was used in the subsequent reaction without isolation procedures further.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08202677B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-71d2164e01384454a1547b8371ff9982 |
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| 출처 메모 | uspto-grants-2012_06 |
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