Hydrochloric Acid → 3-(Trifluoromethyl)pyrazole
反応式
[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]=1参加物
7
実験手順
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%.
後処理
- temperaturethe mixture was heated
- temperatureto reflux for 4 h
- temperatureto cool
- customThen the mixture was evaporated
- additionToluene was added
- customthe mixture was again evaporated
出典と根拠
- ORDレコード
- ord-d4e4f84c05a14f7987a39cdb0a894bc8
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US09006485B2
反応ノート
読み込み中…