HCID 178511141、化合物 → 1-(2,5-difluorophenyl)-1H-pyrazol-5-amine
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1/[N:9]=[N:10]/[CH2:11][CH2:12][C:13]#[N:14]>[OH-].[Na+]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[N:9]1[C:13]([NH2:14])=[CH:12][CH:11]=[N:10]1参加物
3
実験手順
A mixture of (E)-3-((2,5-difluorophenyl)diazenyl)propanenitrile (710 mg) and 20 mL of 1N NaOH was heated to reflux with stirring for 30 min. The reaction mixture was cooled to ambient temperature and extracted with ether. The ether phase was washed with water, brine, dried over sodium sulfate and filtered through a plug of silica gel. Concentration under vacuum gave 630 mg (88%) of 1-(2,5-difluorophenyl)-1H-pyrazol-5-amine. LCMS (ESI) m+H=196.0; 1H NMR (400 MHz, CDCl3) δ 7.54-7.43 (m, 1H), 7.35-7.00 (m, 3H), 5.63 (d, 1H), 3.96-3.71 (m, 2H).
後処理
- temperaturewas heated
- temperatureto reflux
- extractionextracted with ether
- washThe ether phase was washed with water, brine
- dry with materialdried over sodium sulfate
- filtrationfiltered through a plug of silica gel
- concentrationConcentration under vacuum
出典と根拠
- ORDレコード
- ord-2a7eaf996e2f4a7cb3b01871c1fff527
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US08999998B2
反応ノート
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