Hydrochloric Acid → 3-(Trifluoromethyl)pyrazole
반응식
[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]=1참가 물질
7
실험 절차
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-trifluoromethylpyrazole with a purity of >85%.
후처리
- temperaturethe mixture was heated
- temperatureto reflux for 4 h
- temperatureto cool
- customThen the mixture was evaporated
- additionToluene was added
- customthe mixture was again evaporated
출처 및 근거
- ORD 기록
- ord-4cc1f4e1a6124ddda915f48f3ba7efdc
- 출처 데이터셋
- uspto-grants-2014_12
- 특허 번호
- US08921567B2
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