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

HRID 2392519노트

반응식

HRID 2392519 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-073e8d37d5aa4e2d8cc087ed9f099b74
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05801008

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