4-Chlorophenol → HCID 13254745, Verbindung

HRID 569704Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 569704
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.[Na].[CH3:10][O:11][CH2:12][C:13]([C:16]1([CH2:19][N:20]2[CH:24]=[N:23][CH:22]=[N:21]2)[CH2:18][O:17]1)([CH3:15])[CH3:14]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:18][C:16]([OH:17])([C:13]([CH3:15])([CH3:14])[CH2:12][O:11][CH3:10])[CH2:19][N:20]2[CH:24]=[N:23][CH:22]=[N:21]2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 46844-ChlorophenolHCID 5360545SodiumHCID 132547402-(Methoxy-tert.-butyl)-2-(1,2,4-triazol-1-yl-methyl)-oxirane

Produkt 1

HCID 13254745HCID 13254745, VerbindungAusbeute 64,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

8.1 g (0.0633 mol) of 4-chlorophenol were added to a solution of 0.32 g (0.014 mol) of sodium in 100 ml of absolute ethanol. 10.3 g (0.0488 mol) of 2-(methoxy-tert.-butyl)-2-(1,2,4-triazol-1-yl-methyl)-oxirane, dissolved in 300 ml of absolute ethanol, were added, and the reaction mixture was heated under reflux for 48 hours. The reaction mixture was allowed to cool and was concentrated. The residue was taken up in ethyl acetate, and the solution was washed once with water, once with 1N sodium hydroxide solution, again with water, thereafter with 1N hydrochloric acid and 1N sodium hydroxide solution, again with water, and finally with saturated sodium chloride solution. The organic phase was dried over sodium sulphate, and concentrated. 10.7 g (64.6% of theory) of 2-(4-chlorophenoxymethyl)-3,3-dimethyl-4-methoxy-1-(1,2,4-triazol-1-yl)-butan-2-ol of refractive index nD20 =1.531 were obtained.

Aufarbeitung

  1. additionwere added
  2. temperaturethe reaction mixture was heated
  3. temperatureunder reflux for 48 hours
  4. temperatureto cool
  5. concentrationwas concentrated
  6. washthe solution was washed once with water, once with 1N sodium hydroxide solution, again with water
  7. dry with materialThe organic phase was dried over sodium sulphate
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-b095ca6a6dc5488fb1793341f859723b
Quelldatensatz
uspto-grants-1988_03
Patentnummer
US04734126

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