Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 2-Chloroacrylonitrile | HCID 70198 | — |
| Edukt | 1-Isopropylhydrazine hydrochloride | HCID 85573 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-(propan-2-yl)-1H-pyrazol-3-amine | HCID 19576797 | 58% |
Reaktionsschritte
2-Chloroacrylonitrile (3.41 mL, 42.59 mmol) was added at RT to a stirring solution of N-isopropylhydrazine hydrochloride (4.71 g, 42.6 mmol), potassium carbonate (11.8 g, 85.2 mmol) in water (50 mL). The reaction was warmed to 45° C. for 4 hours before cooling back to RT. The aqueous layer was then extracted with ethyl acetate (5×30 mL) and the combined organic layers were dried (MgSO4), treated with activated charcoal, filtered and evaporated. The residue was purified by chromatography, eluting with 67%-100% ethyl acetate in hexanes, to afford the title compound (3.08 g, 58%) as a 6:1 mixture of authentic product to regioisomeric product as an oil. The material was used without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US07745475B2 |
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| Quelldatensatz | uspto-grants-2010_06 |
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| ORD ID | ord-3d1941a623324da78a0d203e0cbd8d49 |
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| Quellennotiz | uspto-grants-2010_06 |
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