Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 1-(5-Trifluoromethyl-pyridin-2-yl)-piperazine | HCID 667618 | — |
| Edukt | 3-[6-Chloro-5-phenyl-2-(trifluoromethyl)pyrimidin-4-yl]benzenesulfonamide | HCID 86613621 | — |
| Lösungsmittel | Pyridine | HCID 1049 | — |
| Produkt | HCID 25004369 | HCID 25004369 | — |
Reaktionsschritte
A solution of 3-[6-chloro-5-phenyl-2-(trifluoromethyl)pyrimidin-4-yl]benzenesulfonamide (0.1 g, 0.242 mmol) in pyridine (2 ml) was treated with 1-[5-(trifluoromethyl)pyridin-2-yl]piperazine (0.3 g, 0.68 mmol) and the reaction mixture was stirred for 1 hour at room temperature. Subsequently the reaction mixture was poured onto crushed ice containing two drops of concentrated hydrochloric acid, extracted with ethyl acetate (25 ml) and the organic layer was washed with brine and evaporated. The title compound was obtained by column chromatographic purification of the crude material with 30% ethyl acetate in hexane. 1H-NMR (DMSO-d6) δ: 3.33-3.37 (m, 4H), 3.56 (m, 4H), 6.86-6.88 (d, 1H), 7.10-7.12 (d, 2H), 7.22-7.29 (m, 3H), 7.35-7.37 (m, 1H), 7.44-7.48 (m, 1H), 7.74-7.79 (m, 3H), 8.38 (s, 1H); MS m/z: 608.8 (M+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08828999B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-a240d3e678cf43de9dd5c77babba9180 |
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| Quellennotiz | uspto-grants-2014_09 |
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