Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dimethyl Sulfoxide | HCID 679 | — |
| Edukt | 2',4'-Dichloroacetophenone | HCID 16693 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | Trimethylsulfonium iodide | HCID 75127 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 2-(2,4-Dichlorophenyl)-2-methyloxirane | HCID 19992437 | — |
Reaktionsschritte
DMSO is added to NaH (1-1.8 equiv.) and heated to 65° C. for one h. THF is added at same temperature and heated for another 10 min. After 10 min., the reaction mixture is cooled to 0° C. Trimethylsulfonium iodide (1-1.2 equiv.) is added and the contents are stirred for 10 min. after which the solution of 1-(2,4-dichlorophenyl)ethanone (1 equiv.) in THF is added dropwise. After complete addition, the reaction mixture is stirred at RT for 2 h; the reaction is monitored by LCMS. After completion, the reaction mixture is poured in ice water, extracted in diethyl ether, dried over sodium sulfate and concentrated at 25° C. to get the crude product.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08907097B2 |
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| Quelldatensatz | uspto-grants-2014_12 |
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| ORD ID | ord-a374ba833f1e474899746d20a51b0048 |
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| Quellennotiz | uspto-grants-2014_12 |
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