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Sulfuric Acid → 1H-Pyrazole, 1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-3,5-dimethyl-

HRID 1031156
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반응식

HRID 1031156 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[NH:13][NH2:14].[CH3:15][C:16](=O)[CH2:17][C:18](=O)[CH3:19].S(=O)(=O)(O)O>C(O)C>[CH3:15][C:16]1[CH:17]=[C:18]([CH3:19])[N:13]([C:3]2[C:2]([Cl:1])=[CH:7][C:6]([C:8]([F:9])([F:11])[F:10])=[CH:5][C:4]=2[Cl:12])[N:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 31261AcetylacetoneHCID 688223[2,6-Dichloro-4-(trifluoromethyl)phenyl]hydrazine

생성물 1

HCID 27410921H-Pyrazole, 1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-3,5-dimethyl-

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 2,6-dichloro-4-trifluoromethylphenylhydrazine (5.0 g), 2,4-pentanedione (2.1 ml) and conc. sulphuric acid (0.8 ml) in ethanol (40 ml) was heated under reflux for 20 hours. The ethanol was evaporated under reduced pressure and the residue dissolved in dichloromethane. The extract was washed with sodium bicarbonate solution and brine, dried over magnesium sulphate and evaporated to give 3,5-dimethyl-1-(2,6-dichloro-4-trifluoromethylphenyl)-1H-pyrazole.

후처리

  1. temperatureunder reflux for 20 hours
  2. customThe ethanol was evaporated under reduced pressure
  3. dissolutionthe residue dissolved in dichloromethane
  4. washThe extract was washed with sodium bicarbonate solution and brine
  5. dry with materialdried over magnesium sulphate
  6. customevaporated

출처 및 근거

ORD 기록
ord-cd9290ee10e949e2acaef56d7e03cabe
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05109012

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