Реакция #316238

ord-445e422ad73a45c0842593b7dbbf6241

Растворители

Условия реакции

Температура
140°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction solution was cooled to room temperature
  2. 2
    Экстракцияthe mixture was extracted with ethyl acetate
  3. 3
    ПромывкаThe ethyl acetate layer was washed with water
  4. 4
    Сушкаwas dried over anhydrous sodium sulfate
  5. 5
    ДругоеThe solvent was removed by distillation under the reduced pressure
  6. 6
    Другоеthe residue was purified by thin layer chromatography

Методика

Dimethyl sulfoxide (2 ml) was added to 5,6,5′-trimethyl-[2,2′]bipyridin-3-ol (50 mg), 4,7-dichloroquinoline (139 mg), and cesium carbonate (228 mg), and the mixture was stirred at 140° C. for 5 hr. The reaction solution was cooled to room temperature, water was then added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give the title compound (77 mg, yield 94%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07560558B2uspto-grants-2009_07