Hydrazine hydrate (1:1) → Bay-H-1127

HRID 502935

反応式

HRID 502935 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 16736Bay-H-1127

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-958bd81a35f8429eb342cc6ebbb51120
出典データセット
uspto-grants-2010_08
特許番号
US07776884B2

関連ノート

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