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

HRID 1865206

Reaktionsgleichung

Reaktionsgleichung von HRID 1865206
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

Komponenten

3

Edukt 2

HCID 6061MethylhydrazineHCID 27346752-Fluoro-4-hydroxybenzonitrile

Produkt 1

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

Versuchsvorschrift

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.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-7ee42ce26a8c4b26a8c3756bbd828c1a
Quelldatensatz
uspto-grants-2009_12
Patentnummer
US07626030B2

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