Реакция #45642

ord-8219cbd171274518809f772ead8ce063

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONcarbon-held palladium catalyst (5% wet, 580 mg) was added
  2. 2
    ДругоеAfter the reaction
  3. 3
    Другоеthe insoluble matter was separated by filtration through Celite
  4. 4
    Концентрированиеthe filtrate was concentrated under reduced pressure
  5. 5
    ДругоеThe resulting residue was recrystallized
  6. 6
    Другоеpurified with n-hexane/ethyl acetate

Методика

N-(4-Bromo-2-cyano-5-fluoro-6-hydroxy-3-methylphenyl)-2,2-dimethyl-3-[(phenylmethyl)oxy]propionamide (I-105) (5.82 g, 13.37 mmol) was dissolved in ethyl acetate (120 ml), carbon-held palladium catalyst (5% wet, 580 mg) was added, followed by vigorously stirring at room temperature under atmospheric pressure of hydrogen for 18 hours. After the reaction, the insoluble matter was separated by filtration through Celite, the filtrate was concentrated under reduced pressure. The resulting residue was recrystallized and purified with n-hexane/ethyl acetate to obtain the entitled compound (2.32 g, 50%) as a white solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07737166B2uspto-grants-2010_06