Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Chlorotrimethylsilane | HCID 6397 | — |
| Edukt | Chlorobenzene | HCID 7964 | — |
| Edukt | Diphenyl sulfoxide | HCID 13679 | — |
| Edukt | Magnesium | HCID 5462224 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Triphenylsulfonium chloride | HCID 61343 | — |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08202677B2 |
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| Quelldatensatz | uspto-grants-2012_06 |
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| ORD ID | ord-71d2164e01384454a1547b8371ff9982 |
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| Quellennotiz | uspto-grants-2012_06 |
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