HCID 178511141, 화합물 → 1-(2,5-difluorophenyl)-1H-pyrazol-5-amine
반응식
[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]1참가 물질
3
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-2a7eaf996e2f4a7cb3b01871c1fff527
- 출처 데이터셋
- uspto-grants-2015_04
- 특허 번호
- US08999998B2
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