Hydrazine → 5-ethyl-3-(trifluoromethyl)-1H-pyrazole
Reaktionsgleichung
[F:1][C:2]([F:11])([F:10])[C:3](=O)[CH2:4][C:5](=O)[CH2:6][CH3:7].[NH2:12][NH2:13]>C(O)C>[CH2:6]([C:5]1[NH:13][N:12]=[C:3]([C:2]([F:11])([F:10])[F:1])[CH:4]=1)[CH3:7]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a solution of 1,1,1-Trifluoro-hexane-2,4-dione (1 g, 5.95 mmol) in absolute ethanol (10 mL) was added NH2NH2.xH2O drop-wise at 0° C. The reaction mixture warmed to the room temperature during 1 hour and refluxed overnight. Ethanol was then evaporated, residue dissolved in ethyl acetate (20 mL), washed consecutively with saturated brine solution and water, dried with Na2SO4 and concentrated to give the title compound as colorless oil.
Aufarbeitung
- customat 0° C
- temperaturerefluxed overnight
- customEthanol was then evaporated
- dissolutionresidue dissolved in ethyl acetate (20 mL)
- washwashed consecutively with saturated brine solution and water
- dry with materialdried with Na2SO4
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-81688da026a44ce7882e623d55ee89df
- Quelldatensatz
- uspto-grants-2007_01
- Patentnummer
- US07157464B2
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