Reaktion #1857547

ord-a0f60c01467e4bb49e4d352d2ae3b07f

Reaktionsgleichung

ClCCl
dichloro methane
[H-].[Na+]
sodium hydride
C=CC(O)(Cn1cncn1)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
2-[2-chloro-4-(4-chlorophenoxy)phenyl]-1-(1,2,4-triazol-1-yl)but-3-en-2-ol
CI
methyl iodide
C=CC(Cn1cncn1)(OC)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
desired compound
C=CC(Cn1cncn1)(OC)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
1-[2-[2-chloro-4-(4-chlorophenoxy)phenyl]-2-methoxy-but-3-enyl]-1,2,4-triazole

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was then heated for 10 h
  2. 2
    Temperaturto reflux
  3. 3
    Sonstigethe organic phase was dried
  4. 4
    Sonstigeevaporated
  5. 5
    Sonstigeto obtain the crude product
  6. 6
    SonstigeThis was purified by column chromatography

Vorschrift

2-[2-chloro-4-(4-chlorophenoxy)phenyl]-1-(1,2,4-triazol-1-yl)but-3-en-2-ol (0.4 g) was dissolved in THF (10 mL) and sodium hydride (0.03 g) was added. The mixture was stirred for 30 min at room temperature and methyl iodide (0.08 mL) was added. The mixture was then heated for 10 h to reflux. Brine and dichloro methane were added, the organic phase was dried and evaporated to obtain the crude product. This was purified by column chromatography to obtain 0.04 g of the desired compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09247747B2uspto-grants-2016_02