Реакция #88859

ord-4c24d83293bb4de397e1430573d9cf87

Растворители

Условия реакции

Температура
150°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияthe mixture was extracted with ethyl acetate
  2. 2
    ПромывкаThe extract was washed with saturated brine
  3. 3
    Сушкаdried over anhydrous sodium sulfate
  4. 4
    ДругоеThe solvent was evaporated under reduced pressure
  5. 5
    ДругоеThe residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane)

Методика

A mixture of (4-benzyl-4-hydroxypiperidin-1-yl) (5-bromo-1,3-benzodioxol-4-yl)methanone (0.50 g), pyridine-4-boronic acid (0.22 g), sodium carbonate (0.38 g), tetrakis(triphenylphosphine)palladium(0) (0.069 g), water (0.50 mL) and DME (2.5 mL) was stirred at 150° C. for 1 hr under microwave irradiation. The reaction mixture was diluted with water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, ethyl acetate/hexane) to give the title compound (0.85 g).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09440990B2uspto-grants-2016_09