Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 3-Chloro-4-(trifluoromethyl)phenol | HCID 13609147 | — |
| Edukt | 5-chloro-2,4-difluoro-N-(methylsulfonyl)benzamide | HCID 58042417 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | HCID 56592534 | HCID 56592534 | 4,9% |
Reaktionsschritte
To 3-chloro-4-(trifluoromethyl)phenol (Preparation 16, 110 mg, 0.56 mmol) and 5-chloro-2,4-difluoro-N-(methylsulfonyl)benzamide (Preparation 13, 150 mg, 0.56 mmol) dissolved in dimethylsulfoxide (5 ml) was added potassium carbonate (232 mg, 1.68 mmol) and the mixture stirred at 90° C. for 18 hours under nitrogen. The mixture was poured onto ammonium chloride (aq) and extracted with ethyl acetate (3×20 mL), washed with water (3×20 mL) and dried (MgSO4). Purification of the crude product by silica gel column chromatography using 80% Ethyl acetate in heptane furnished the title compound as white solid (12.2 mg, 4.9%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08685977B2 |
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| Quelldatensatz | uspto-grants-2014_04 |
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| ORD ID | ord-8bee4fb434a64faeb7dd7f8f9e37ae79 |
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| Quellennotiz | uspto-grants-2014_04 |
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