Methylhydrazine → 3-amino-1-methyl-1H-indazol-6-ol

HRID 1865206

반응식

HRID 1865206 반응식
F[C:2]1[C:7]([C:8]#[N:9])=[CH:6][CH:5]=[C:4]([OH:10])[CH:3]=1.[CH3:11][NH:12][NH2:13]>>[NH2:9][C:8]1[C:7]2[C:2](=[CH:3][C:4]([OH:10])=[CH:5][CH:6]=2)[N:12]([CH3:11])[N:13]=1

참가 물질

3

반응물 2

HCID 6061MethylhydrazineHCID 27346752-Fluoro-4-hydroxybenzonitrile

생성물 1

HCID 1357424603-amino-1-methyl-1H-indazol-6-ol

실험 절차

A solution of 6-fluoro-4-hydroxy benzonitrile (Aldrich, 10.1 g, 73.9 mmol) in methyl hydrazine (Aldrich, 20.0 mL, 379 mmol) was stirred at 80° C. for 16 h. After cooling to RT, the volatile portion was removed in vacuo. The residue was triturated with DCM and MeOH. The title compound was obtained by filtration as an off-white solid. The filtrate was concentrated in vacuo and purified by silica gel chromatography (DCM/MeOH: 100/0 to 95/5) to give an additional amount of the title compound as a white solid.

후처리

  1. customthe volatile portion was removed in vacuo
  2. customThe residue was triturated with DCM and MeOH

출처 및 근거

ORD 기록
ord-7ee42ce26a8c4b26a8c3756bbd828c1a
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07626030B2

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