Reaktion #507646

ord-a47570c8e78d4503a532690758bebbc3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwith heating for 7 hours
  2. 2
    SonstigeAfter completion of the reaction
  3. 3
    Waschenwashed with water
  4. 4
    Trocknendried with sodium sulfate
  5. 5
    SonstigeRemoving the solvent
  6. 6
    workup.DISTILLATIONby distillation

Vorschrift

Dissolving 1.2 g (3.4 mmol) of 1-(4-bromophenyl)-2-pyridine-2-yl-1H-benzimidazole, 1.2 g (3.4 mmol) of 10-naphthalene-2-yl-anthracene-9-boronic acid and 0.10 g of tetrakis (triphenylphosphine) palladium into 15 milliliter of 1,2-dimethoxyethane, adding 6 milliliter of 2.0M sodium carbonate aqueous solution, the resultant suspension was refluxed with heating for 7 hours. After completion of the reaction, the precipitated solids were dissolved into the dichloro-methane, washed with water and dried with sodium sulfate. Removing the solvent by distillation and by refining the resultant product with the use of a silicagel column chromatography (dichloro methane-ethyl acetate), 1.2 g of an yellowish white solids were obtained (yield: 61%). As a result of MS analysis, it was recognized that the yellowish white solids were identified as the aimed substance and that m/e=573 for molecular weight of 573.22.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08097349B2uspto-grants-2012_01