Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Lithium Hydroxide | HCID 3939 | — |
| Edukt | Sodium Iodide | HCID 5238 | — |
| Edukt | 2-tert-Butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-cyclopropyl-pyrimidine | HCID 69026125 | — |
| Edukt | HCID 178481704 | HCID 178481704 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | Hydrochloric Acid | HCID 313 | — |
| Produkt | 2-tert-Butyl-4-{4-[3-(4-methyl-5-trifluoromethyl-4H-[1,2,4]triazol-3-ylsulfanyl)-propyl]-piperazin-1-yl}-6-cyclopropyl-pyrimidine hydrochloride | HCID 69025984 | — |
Reaktionsschritte
0.3 g of 2-tert-Butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-cyclopropyl-pyrimidine (0.89 mmol) were dissolved in 10 ml dimethylformamide. After the addition of 0.163 g 4-Methyl-5-trifluoromethyl-4H-[1,2,4]triazole-3-thiol (0.89 mmol), 0.064 g lithium hydroxide (2.76 mmol) and 0.067 g sodium iodide (0.45 mmol), the reaction mixture was stirred at 78° C. for 3 h. After cooling, the solvent was evaporated and the residue was dissolved in 30 ml of ethyl acetate. After washing twice with water, the organic phase was dried over magnesium sulfate, filtered, and the solvent was evaporated. The residue was purified chromatography on silica gel with ethyl acetate. Fractions containing the product were combined and the solvent was evaporated. The hydrochloride was formed by addition of 4 N HCl in dioxan to yield 0.14 g of the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08202868B2 |
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| Quelldatensatz | uspto-grants-2012_06 |
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| ORD ID | ord-0af4c1f2cb5c4731b81f62785483dac5 |
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| Quellennotiz | uspto-grants-2012_06 |
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