Phenylhydrazine → 5-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile

HRID 68718

반응식

HRID 68718 반응식
[C:1]1([NH:7][NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(O[C:12](=[C:14]([C:17]#[N:18])[C:15]#[N:16])[CH3:13])C.C(OC=C(C#N)C#N)C>C(O)C>[NH2:18][C:17]1[N:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:8]=[C:12]([CH3:13])[C:14]=1[C:15]#[N:16]

참가 물질

5

반응물 3

HCID 7516PhenylhydrazineHCID 671522-(Ethoxymethylene)propanedinitrileHCID 79450(1-Ethoxyethylidene)malononitrile

생성물 1

HCID 2198585-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Into a 250-mL 3-necked round-bottom flask, was placed a solution of 1-phenylhydrazine (31.5 g, 291.67 mmol, 1.14 equiv) in ethanol (105 mL) at room temperature. To the resulting mixture was then added 2-(1-ethoxyethylidene)malononitrile (35 g, 257.35 mmol, 1.00 equiv) in several batches at room temperature. After about half of the addition was completed, the solution was carefully heated to boiling. After all the ethoxymethylene malononitrile was added, the resulting solution was heated to reflux for 4 hr. The resulting mixture was then cooled with a water/ice bath, and the solids were collected by filtration to yield 5-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile as a yellow solid.

후처리

  1. customInto a 250-mL 3-necked round-bottom flask, was placed
  2. customat room temperature
  3. customat room temperature
  4. additionAfter about half of the addition
  5. temperaturethe solution was carefully heated to boiling
  6. temperaturethe resulting solution was heated
  7. temperatureto reflux for 4 hr
  8. temperatureThe resulting mixture was then cooled with a water/ice bath
  9. filtrationthe solids were collected by filtration

출처 및 근거

ORD 기록
ord-f135ab60af0c414f928bdb7fa3b2c11f
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822447B2

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