1H-1,2,4-Triazole → 4-(2,4-Dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butanone

HRID 979458

Reaktionsgleichung

Reaktionsgleichung von HRID 979458
Br[CH2:2][C:3](=[O:16])[C:4]([CH3:15])([CH3:14])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][C:7]=1[Cl:13].[NH:17]1[CH:21]=[N:20][CH:19]=[N:18]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[Cl:13][C:7]1[CH:8]=[C:9]([Cl:12])[CH:10]=[CH:11][C:6]=1[CH2:5][C:4]([CH3:15])([CH3:14])[C:3](=[O:16])[CH2:2][N:17]1[CH:21]=[N:20][CH:19]=[N:18]1

Komponenten

5

Edukt 3

HCID 92571H-1,2,4-TriazoleHCID 11430Potassium CarbonateHCID 133403811-Bromo-4-(2,4-dichlorophenyl)-3,3-dimethyl-2-butanone

Produkt 1

HCID 133403824-(2,4-Dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butanoneAusbeute 45,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

30 g (0.09 mole) of 1-bromo-4-(2,4-dichlorophenyl)-3,3-dimethyl-2-butanone, 12.4 g (0.18 mole) of 1,2,4-triazole and 24.8 g (0.18 mole) of potassium carbonate in 300 ml of acetone are heated under reflux for 6 hours. The mixture is then allowed to cool, the solid is filtered off with suction and the mother liquor is evaporated in vacuo. The residue is taken up in methylene chloride, and the solution is washed with water, dried over sodium sulphate and evaporated in vacuo. The residue is recrystallised from diethyl ether. 12.8 g (45.6% of theory) of 4-(2,4-dichlorophenyl)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-2-butanone of melting point 85° C. are obtained.

Aufarbeitung

  1. temperatureunder reflux for 6 hours
  2. temperatureto cool
  3. filtrationthe solid is filtered off with suction
  4. customthe mother liquor is evaporated in vacuo
  5. washthe solution is washed with water
  6. dry with materialdried over sodium sulphate
  7. customevaporated in vacuo
  8. customThe residue is recrystallised from diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-b7de8dbd764244a89d31f25d6fa42932
Quelldatensatz
uspto-grants-1987_05
Patentnummer
US04668660

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