Phenylhydrazine → 5-Amino-3-(methylsulfanyl)-1-phenyl-1H-pyrazole-4-carbonitrile

HRID 2392519ノート

反応式

HRID 2392519 の反応式
CS[C:3](=[C:6]([C:9]#[N:10])[C:7]#[N:8])[S:4][CH3:5].[C:11]1([NH:17][NH2:18])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>C(O)C>[NH2:8][C:7]1[N:17]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:18]=[C:3]([S:4][CH3:5])[C:6]=1[C:9]#[N:10]

参加物

4

反応物 2

HCID 7516PhenylhydrazineHCID 992292-(Bis(methylsulfanyl)methylidene)propanedinitrile

生成物 1

HCID 7367765-Amino-3-(methylsulfanyl)-1-phenyl-1H-pyrazole-4-carbonitrile収率 91%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture comprised of 17.0 g (100 mmol) of bis (methylthio)methylenepropanedinitrile, 10.8 g (100mmol) of phenylhydrazine and 80 ml of ethanol was heated under reflux for 2 hours. The solvent was removed through distillation, and 20 ml of ethanol was added to the residue, which was thus crystallized. The resulting crystals were taken out by means of filtration under suction to give 20.9 g (9.1 mmol) of the entitled product as colorless, needle-like crystals having a melting point of from 136° to 137° C. The yield was 91%.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. customThe solvent was removed through distillation, and 20 ml of ethanol
  4. additionwas added to the residue, which
  5. customwas thus crystallized
  6. filtrationThe resulting crystals were taken out by means of filtration under suction

出典と根拠

ORDレコード
ord-073e8d37d5aa4e2d8cc087ed9f099b74
出典データセット
uspto-grants-1998_09
特許番号
US05801008

反応ノート

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