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Hydrogen Peroxide → HCID 487678, Verbindung

HRID 611815
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 611815
[F:1][C:2]([F:21])(SC)[C:3]([C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=1[F:18])([OH:10])[CH2:4][N:5]1[CH:9]=[N:8][CH:7]=[N:6]1.OO.[S:24]([O-:28])([O-])(=[O:26])=S.[Na+].[Na+].[CH3:31]O>O.O.[O-][W]([O-])(=O)=O.[Na+].[Na+]>[F:21][C:2]([F:1])([S:24]([CH3:31])(=[O:28])=[O:26])[C:3]([C:11]1[CH:16]=[CH:15][C:14]([F:17])=[CH:13][C:12]=1[F:18])([OH:10])[CH2:4][N:5]1[CH:9]=[N:8][CH:7]=[N:6]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 784Hydrogen PeroxideHCID 887MethanolHCID 24477Sodium ThiosulfateHCID 10853188HCID 10853188, Verbindung

Produkt 1

HCID 487678HCID 487678, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 150191Sodium Tungstate Dihydrate
Katalysator

Versuchsvorschrift

To a 10 ml solution of 0.50 g (1.6 mol) of 3,3-difluoro-2-(2',4'-difluorophenyl)-3-methylthio-1-(1H-1,2,4-triazole-1-yl)-propan-2-ol [Compound (1a-1)] in methanol, 0.01 g (0.03 mmol) of sodium tungstate dihydrate was added, followed by the dropwise addition of 0.53 g (4.7 mmol) of a 30% aqueous solution of hydrogen peroxide at room temperature under stirring. The resulting mixture was stirred at room temperature for 16 hours. To the reaction mixture, a 10% aqueous solution of sodium thiosulfate was added to decompose an excess oxidizing agent. Methanol was then distilled off under reduced pressure. To the residue, chloroform was added, followed by washing successively with water and saturated saline and drying over anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure. The crystals so precipitated were recrystallized from chloroform, whereby 8.0 g of the title Compound (1c-1) were obtained in the form of colorless crystals (yield: 74%).

Aufarbeitung

  1. stirringThe resulting mixture was stirred at room temperature for 16 hours
  2. distillationMethanol was then distilled off under reduced pressure
  3. additionTo the residue, chloroform was added
  4. washby washing successively with water and saturated saline
  5. dry with materialdrying over anhydrous magnesium sulfate
  6. distillationThe solvent was then distilled off under reduced pressure
  7. customThe crystals so precipitated
  8. customwere recrystallized from chloroform

Quellen und Nachweise

ORD-Eintrag
ord-f65f08cefe2247aaab50c8f526294a96
Quelldatensatz
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06002028

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