Hydrochloric Acid → 3-(Trifluoromethyl)pyrazole
Reaktionsgleichung
[F:1][C:2]([F:10])([F:9])[C:3](=O)[CH:4]=[CH:5]OC.Cl.O.[NH2:13][NH2:14].[OH-].[Na+]>O.C(O)C>[F:1][C:2]([F:10])([F:9])[C:3]1[CH:4]=[CH:5][NH:14][N:13]=1Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
2.71 kg of 1,1,1-trifluoro-4-methoxy-but-3-en-2-on, 2.44 kg of ethanol and 3.10 kg of water were charged into a reaction vessel. 20 ml of concentrated hydrochloric acid and 0.80 kg of hydrazine hydrate were successively added and the mixture was heated to reflux for 4 h. The mixtures was allowed to cool and neutralized by addition of 10% aqueous NaOH to about pH 4-5. Then the mixture was evaporated. Toluene was added and the mixture was again evaporated to yield 2 kg of raw 3-trifluoromethyl-pyrazole with a purity of >85%.
Aufarbeitung
- temperaturethe mixture was heated
- temperatureto reflux for 4 h
- temperatureto cool
- customThen the mixture was evaporated
- additionToluene was added
- customthe mixture was again evaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-0d5fea2d65da4550b380123ef28fb807
- Quelldatensatz
- uspto-grants-2016_03
- Patentnummer
- US09282741B2
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