Реакция #90092

ord-f865c7d0fe7f44da81d69c156db8f76c

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted with ethyl acetate
  2. 2
    Экстракцияextracted with ethyl acetate
  3. 3
    Промывкаwashed with saturated brine
  4. 4
    Сушкаdried over sodium sulfate
  5. 5
    ДругоеThe drying agent was removed by filtration
  6. 6
    Другоеthe residues obtained
  7. 7
    Концентрированиеafter concentration under reduced pressure
  8. 8
    Другоеwere purified by silica gel column chromatography (ethyl acetate/hexane)
  9. 9
    Другоеto obtain the target compound (white solid, 1.10 g, 84%)

Методика

2-(4-Isopropoxy-3-methoxy-phenyl)-2-methyl-propionic acid ethyl ester (Compound L3-1, 1.45 g, 5.17 mmol) was dissolved in THF (13 mL) and EtOH (13 mL), added with 1 N aqueous solution of sodium hydroxide (10.3 mL, 2.0 eq.), and stirred at 80° C. overnight. The reaction solution was added to water and extracted with ethyl acetate. The aqueous layer was acidified by using 1 N aqueous solution of hydrochloric acid, extracted with ethyl acetate, washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the target compound (white solid, 1.10 g, 84%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09440922B2uspto-grants-2016_09