Phenylhydrazine → 5-Amino-3-methyl-1-phenylpyrazole

HRID 68734

Reaktionsgleichung

Reaktionsgleichung von HRID 68734
O=[C:2]([CH3:6])[CH2:3][C:4]#[N:5].[C:7]1([NH:13][NH2:14])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)C>[CH3:6][C:2]1[CH:3]=[C:4]([NH2:5])[N:13]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:14]=1

Komponenten

4

Versuchsvorschrift

Into a 1000-mL 3-necked round bottom flask, was placed a solution of 3-oxobutanenitrile (23 g, 277.11 mmol, 1.00 equiv) in ethanol (400 mL), 1-phenylhydrazine (30 g, 277.78 mmol, 1.00 equiv). The resulting solution was heated to reflux overnight in an oil bath. The resulting mixture was then concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:10-1:5) to yield 3-methyl-1-phenyl-1H-pyrazol-5-amine as a yellow solid.

Aufarbeitung

  1. customInto a 1000-mL 3-necked round bottom flask, was placed
  2. temperatureThe resulting solution was heated
  3. temperatureto reflux overnight in an oil bath
  4. concentrationThe resulting mixture was then concentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-afa94241a6334361b469a8216d898f9c
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822447B2

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