Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethanol | HCID 702 | — |
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-1H-pyrazole | HCID 86694306 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 86694305 | HCID 86694305 | 91,3% |
Reaktionsschritte
To a mixture of 980 mg of 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-1H-pyrazole, 9.8 mL of tetrahydrofuran, 19.6 mL of ethanol, and 2.9 mL of water was added 102 mg of ammonium chloride, followed by heating at 70° C. 1.03 g of reduced iron was added thereto, followed by heating to reflux for 4 hours, and cooling to room temperature. The insoluble material was filtered through celite, the filtrate was concentrated, and a mixture of chloroform/water was added thereto. The aqueous layer was separated, and then the organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to obtain 815 mg of 5-bromo-2-(1-cyclopentyl-1H-pyrazol-5-yl)aniline.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08822448B2 |
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| Quelldatensatz | uspto-grants-2014_09 |
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| ORD ID | ord-f3c6bf8d61d947d2812926e39b822455 |
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| Quellennotiz | uspto-grants-2014_09 |
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