Hydrochloric Acid → 1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-amine
反応式
[CH3:1][NH:2][NH2:3].[F:4][C:5]([F:12])([F:11])[C:6](=O)[CH2:7][C:8]#[N:9].Cl>CCO>[CH3:1][N:2]1[C:8]([NH2:9])=[CH:7][C:6]([C:5]([F:12])([F:11])[F:4])=[N:3]1参加物
5
実験手順
A solution of methylhydrazine (5.0 g, 60 mmol) and 4,4,4-trifluoro-3-oxo-butyronitrile (9.8 g, 71 mmol) in EtOH (50 mL) was treated with conc. HCl (5 mL) and the resultant mixture was heated to reflux overnight. The solvent was removed in vacuo and the crude product was dissolved in EtOAc washed with saturated aq. Na2CO3 solution until the washings were pH 8. The organics were concentrated and purified by prep-HPLC to provide 2-methyl-5-trifluoromethyl-2H-pyrazol-3-ylamine (2.07 g, 21% yield). 1H NMR (300 MHz, DMSO-d6), δ 5.57 (s, 1 H), 5.54 (br s, 2 H), 3.55 (s, 3 H); MS (ESI) m/z: 166.1 (M+H+).
後処理
- temperatureto reflux overnight
- customThe solvent was removed in vacuo
- dissolutionthe crude product was dissolved in EtOAc
- washwashed with saturated aq. Na2CO3 solution until the washings
- concentrationThe organics were concentrated
- custompurified by prep-HPLC
出典と根拠
- ORDレコード
- ord-4c3c327c0ab04c749843ef49eaf5136a
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08143293B2
反応ノート
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