Hydrazine hydrate (1:1) → Bay-H-1127

HRID 502935

반응식

HRID 502935 반응식
F[C:2]1[CH:9]=[CH:8][C:7]([C:10]([F:13])([F:12])[F:11])=[CH:6][C:3]=1[C:4]#[N:5].[NH2:14][NH2:15].O>CCCCO>[F:11][C:10]([F:12])([F:13])[C:7]1[CH:6]=[C:3]2[C:2](=[CH:9][CH:8]=1)[NH:15][N:14]=[C:4]2[NH2:5]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 5210162-Fluoro-5-(trifluoromethyl)benzonitrile

생성물 1

HCID 16736Bay-H-1127

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

2-Fluoro-5-trifluoromethyl-benzonitrile (2.66 g) was dissolved in n-BuOH (51 ml) prior to the addition of NH2NH2.H2O (1.02 ml). The solution was heated to reflux for 30 min. After cooling to rt, the solution was concentrated and CH2Cl2 was added. The organic layer was washed with H2O, brine, dried, filtered, and concentrated in high vacuum to give 5-trifluoromethyl-1H-indazol-3-ylamine (2.25 g): 1H NMR (DMSO, δppm, 300 mHz) 5.70 (s, br, 2H), 7.40 (dd, 2H), 8.20 (s, 1H), 11.90 (s, br, 1H).

후처리

  1. temperatureThe solution was heated
  2. temperatureto reflux for 30 min
  3. concentrationthe solution was concentrated
  4. additionCH2Cl2 was added
  5. washThe organic layer was washed with H2O, brine
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated in high vacuum

출처 및 근거

ORD 기록
ord-958bd81a35f8429eb342cc6ebbb51120
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776884B2

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