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

HRID 1865206

反応式

HRID 1865206 の反応式
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

参加物

3

反応物 2

HCID 6061MethylhydrazineHCID 27346752-Fluoro-4-hydroxybenzonitrile

生成物 1

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

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-7ee42ce26a8c4b26a8c3756bbd828c1a
出典データセット
uspto-grants-2009_12
特許番号
US07626030B2

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