Reaktion #41532

ord-5739102b7b02496e84958cd0c1d66046

Reaktionsgleichung

c1nc[nH]n1
[1,2,4]triazole
[H-].[Na+]
sodium hydride
CN(C)C=O
dimethylformamide
CS(=O)(=O)c1nc2c(Oc3ccc(F)cc3)cc(Oc3cccnc3)cc2[nH]1
4-(4-fluoro-phenoxy)-2-methanesulfonyl-6-(pyridin-3-yloxy)-1H-benzimidazole
Fc1ccc(Oc2cc(Oc3cccnc3)cc3[nH]c(-n4cncn4)nc23)cc1
4-(4-fluoro-phenoxy)-6-(pyridin-3-yloxy)-2-[1,2,4]triazol-1-yl-1H-benzimidazole

Lösungsmittel

Reaktionsbedingungen

Temperatur
160°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe reaction liquid
  2. 2
    SonstigeThe reaction liquid
  3. 3
    Waschenwashed with water and saturated saline in order
  4. 4
    Trocknendried with anhydrous magnesium sulfate
  5. 5
    SonstigeThe solvent was evaporated away under reduced pressure
  6. 6
    Sonstigethe resulting residue was purified
  7. 7
    Sonstigethrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), ethyl acetate)
  8. 8
    Sonstigeto obtain the entitled compound

Vorschrift

5.0 mg of sodium hydride was added to a dimethylformamide (0.5 ml) solution of 16 mg of 4-(4-fluoro-phenoxy)-2-methanesulfonyl-6-(pyridin-3-yloxy)-1H-benzimidazole, and then 10.4 mg of [1,2,4]triazole was added to it, and the reaction liquid was stirred overnight at 160° C. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), ethyl acetate) to obtain the entitled compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728025B2uspto-grants-2010_06