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

HRID 68734

反応式

HRID 68734 の反応式
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

参加物

4

反応物 2

HCID 7516PhenylhydrazineHCID 755793-Oxobutyronitrile

生成物 1

HCID 708015-Amino-3-methyl-1-phenylpyrazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-afa94241a6334361b469a8216d898f9c
出典データセット
uspto-grants-2014_09
特許番号
US08822447B2

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