Reaktion #41528

ord-bb729575983b44119b5762c8c620b5c4

Reaktionsgleichung

S=C=S
carbon disulfide
[K+].[OH-]
potassium hydroxide
CCO
ethanol
Fc1ccc(Oc2cc(Oc3cccnc3)cc3[nH]c(-c4ccccn4)nc23)cc1
3-(4-fluoro-phenoxy)-5-(pyridin-3-yloxy)-benzene-1,2-diamine
Fc1ccc(Oc2cc(Oc3cccnc3)cc3[nH]c(-c4ccccn4)nc23)cc1
4-(4-Fluoro-phenoxy)-2-pyridin-2-yl-6-(pyridin-3-yloxy)-1H-benzimidazole
Fc1ccc(Oc2cc(Oc3cccnc3)cc3[nH]c(S)nc23)cc1
4-(4-fluoro-phenoxy)-6-(pyridin-3-yloxy)-1H-benzimidazole-2-thiol

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°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
    Sonstigeto obtain the entitled compound

Vorschrift

0.06 ml of carbon disulfide and 54 mg of potassium hydroxide were added to an ethanol (2.0 ml) solution of 273 mg of 3-(4-fluoro-phenoxy)-5-(pyridin-3-yloxy)-benzene-1,2-diamine obtained in Example 68, and the reaction liquid was stirred overnight at 80° 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 to obtain the entitled compound.

Quelle

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