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

HRID 68734

반응식

HRID 68734 반응식
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

참가 물질

4

반응물 2

HCID 7516PhenylhydrazineHCID 755793-Oxobutyronitrile

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-afa94241a6334361b469a8216d898f9c
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822447B2

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