Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 2-Chlorostyrene | HCID 14906 | — |
| Edukt | Sodium Hypochlorite | HCID 23665760 | — |
| Edukt | HCID 86631243 | HCID 86631243 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 68745534 | HCID 68745534 | — |
Reaktionsschritte
To a solution of 1-chloro-2-ethenylbenzene (0.035 g, 0.25 mmol), triethylamine (2.5 mg, 0.025 mmol) and Clorox® aqueous sodium hypochlorite solution (1 mL, 16.1 mmol) in dichloromethane (5 mL) was added 4-[4-[(hydroxyimino)methyl]-2-thiazolyl]-1-[[5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]acetyl]piperidine (i.e. the product of Example 2, Step C) (0.10 g, 0.25 mmol) in dichloromethane (5 mL) dropwise over 1 h at 0° C. The reaction mixture was allowed to stir for 1 h, then filtered through Celite® diatomaceous filter aid, and concentrated under reduced pressure to give an oil, which was purified by column chromatography on silica gel using 50% ethyl acetate in hexane as eluant to give 73 mg of the title compound as a white foam, melting at 115-122° C. (crystallized from methyl acetate/petroleum ether).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08642634B2 |
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| Quelldatensatz | uspto-grants-2014_02 |
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| ORD ID | ord-aaf7e68db93d44ffb6098f5868039269 |
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| Quellennotiz | uspto-grants-2014_02 |
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