Hydrochloric Acid → 1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-amine
반응식
[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]1참가 물질
5
실험 절차
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 pre-HPLC to provide 2-methyl-5-trifluoromethyl-2H-pyrazol-3-ylamine (2.07 g, 21% yield). 1HNMR (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+).
후처리
- 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 pre-HPLC
출처 및 근거
- ORD 기록
- ord-67908363196245699605c2f0cfb3fdf1
- 출처 데이터셋
- uspto-grants-2011_03
- 특허 번호
- US07897762B2
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