Ammonium Chloride → HCID 86694716、化合物

HRID 475168ノート

反応式

HRID 475168 の反応式
[F:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[N:7][N:8]2[CH3:11])=[C:4]([C:12](=[N:14]O)[CH3:13])[CH:3]=1.[NH4+].[Cl-]>CO.[Zn]>[F:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[N:7][N:8]2[CH3:11])=[C:4]([CH:12]([NH2:14])[CH3:13])[CH:3]=1

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 136336869HCID 136336869、化合物

生成物 1

HCID 86694716HCID 86694716、化合物収率 99.1%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 887Methanol溶媒

実験手順

To the solution of 1-(6-fluoro-1-methyl-1H-indazol-4-yl)ethanone oxime (848 mg, 4.10 mmol) in MeOH (60 mL) was added powdered Zn (13.6 g, 212.5 mmol, 50.0 eq.) and NH4Cl (13.6 g, 251 mmol, 60.0 eq.). The mixture was heated at reflux overnight, filtered, and concentrated in vacuo. To the residue was added DCM, and the mixture was washed with water, dried (MgSO4) and concentrated in vacuo to afford 1-(6-fluoro-1-methyl-1H-indazol-4-yl)ethanamine (131) as syrup (785 mg, 87%). MS (ESI): m/z=177.2 [M−NH2]+.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux overnight
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. additionTo the residue was added DCM
  6. washthe mixture was washed with water
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-57b4ff46258d4b7eb5640d79dcbec7f2
出典データセット
uspto-grants-2014_01
特許番号
US08637537B2

反応ノート

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