Ammonium Chloride → HCID 86694716, 화합물

HRID 475168노트

반응식

HRID 475168 반응식
[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

참가 물질

5

반응물 2

HCID 25517Ammonium ChlorideHCID 136336869HCID 136336869, 화합물

생성물 1

HCID 86694716HCID 86694716, 화합물수율 99.1%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 887Methanol용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-57b4ff46258d4b7eb5640d79dcbec7f2
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637537B2

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