Reaktion #336543

ord-d0aeda1875dc427da65d412e18833107

Lösungsmittel

Reaktionsbedingungen

Temperatur
20°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted three times with ethyl acetate
  2. 2
    TrocknenThe combined organic phases are dried over magnesium sulfate
  3. 3
    Einengenconcentrated
  4. 4
    SonstigeThe residue is purified by chromatography over silica gel

Vorschrift

5.6 g of p-phenoxyphenol and 4.2 g of potassium carbonate are heated for 1 hour at 70° C. in 50 ml of anhydrous dimethylformamide. Subsequently, 5.6 g of 2-chloro-1-chloromethyl-1,3,4-triazole is added and the mixture stirred for 6 hours at 70° C. and overnight at room temperature (about 20° C.). The mixture is then poured into 500 ml of water and extracted three times with ethyl acetate. The combined organic phases are dried over magnesium sulfate and concentrated. The residue is purified by chromatography over silica gel using n-hexane/ethyl acetate (2:1) as eluant. There is obtained 2.8 g of 2-chloro-1-[(p-phenoxyphenoxy)-methyl]-1,3,4-triazole as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05214064uspto-grants-1993_05