Reacción #41695

ord-789f003969094e3887548f5c03ce85d9

Condiciones de reacción

Temperatura
120°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrothe reaction liquid
  2. 2
    TemperaturaAfter cooled
  3. 3
    Otrothe reaction liquid
  4. 4
    Extracciónextracted with chloroform
  5. 5
    Secadothe organic layer was dried with anhydrous magnesium sulfate
  6. 6
    Otrothe solvent was evaporated away under reduced pressure
  7. 7
    OtroThe resulting residue was purified
  8. 8
    Otrothrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1)

Procedimiento

20 mg of 2-mercaptoethanol and 10 mg of potassium carbonate were added in order to an N,N-dimethylformamide (1 ml) solution of 20 mg of 6-(1-acetylpyrrolidin-2-yl)-5-(6-chloropyridin-3-yl)oxy-2-pyridin-2-yl-1H-benzimidazole obtained in Example 504, and the reaction liquid was stirred at 120° C. for 5 hours. After cooled, the reaction liquid was diluted with aqueous saturated sodium bicarbonate, extracted with chloroform, and the organic layer was dried with anhydrous magnesium sulfate, and the solvent was evaporated away under reduced pressure. The resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1) to obtain the entitled compound as a white solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07728025B2uspto-grants-2010_06