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1H-1,2,4-Triazole → HCID 12765983, Verbindung

HRID 1995925
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1995925
BrBr.[Cl:3][C:4]1[CH:25]=[CH:24][C:7]([O:8][CH2:9][C:10](=[O:23])[C:11]([CH3:22])([CH3:21])[CH2:12][S:13][C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)=[CH:6][CH:5]=1.[NH:26]1[CH:30]=[N:29][CH:28]=[N:27]1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)(Cl)Cl>[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([O:8][CH:9]([N:26]2[CH:30]=[N:29][CH:28]=[N:27]2)[C:10](=[O:23])[C:11]([CH3:21])([CH3:22])[CH2:12][S:13][C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)=[CH:24][CH:25]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 24408BromineHCID 127659751-(4-Chlorophenoxy)-4-(4-chlorophenylmercapto)-3,3-dimethyl-butan-2-one

Produkt 1

HCID 12765983HCID 12765983, VerbindungAusbeute 26 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5943
Carbon Tetrachloride
Lösungsmittel

Versuchsvorschrift

48 g (0.3 mol) of bromine were added dropwise to 110.5 g (0.3 mol) of 1-(4-chlorophenoxy)-4-(4-chlorophenylmercapto)-3,3-dimethyl-butan-2-one in 750 ml of carbon tetrachloride at room temperature. The mixture was subsequently stirred at room temperature for one hour and was concentrated by distilling off the solvent in vacuo, and the residue was taken up in 750 ml of toluene. 73 g (1.06 mol) of 1,2,4-triazole and 150 g (1.06 mol) of potassium carbonate were added to this solution. The mixture was heated to 90° C. for 8 hours and allowed to cool to room temperature and the organic phase was separated off. This phase was extracted with dilute sodium hydroxide solution, rinsed with water, dried over sodium sulphate and concentrated in vacuo. 34 g (26% of theory) of 1-(4-chlorophenoxy)-4-(4-chlorophenylmercapto)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one of melting point 115° C. were obtained.

Aufarbeitung

  1. concentrationwas concentrated
  2. distillationby distilling off the solvent in vacuo
  3. temperatureThe mixture was heated to 90° C. for 8 hours
  4. temperatureto cool to room temperature
  5. customthe organic phase was separated off
  6. extractionThis phase was extracted with dilute sodium hydroxide solution
  7. washrinsed with water
  8. dry with materialdried over sodium sulphate
  9. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b03004be0eab43d6b40fb7c566bc40e4
Quelldatensatz
uspto-grants-1983_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04406909

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