Реакция #1172511

ord-ac68934f827e481a9fb094951a877288

Реагенты

Нет

Растворители

Условия реакции

Температура
87.5°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe reaction is filtered
  2. 2
    Другоеto remove KCl
  3. 3
    Концентрированиеthe filtrate is concentrated under reduced pressure
  4. 4
    Другоеto remove DMF
  5. 5
    workup.DISSOLUTIONThe product is dissolved in ethyl acetate (300 mL)
  6. 6
    Экстракцияextracted with 2N NaOH (2×100 mL) and water (100 mL)
  7. 7
    ДругоеThe organic phase is dried
  8. 8
    Концентрированиеconcentrated

Методика

To a solution of the potassium salt of 4-hydroxyacetophenone (25.0 g, 0.14 mol) in dimethylformamide (DMF) (100 mL) is added methyl 2-chloropropanoate (24.5 g, 0.20 mol) over 30 minutes and stirred at 85-90° C. for 3 hours under nitrogen. The reaction is filtered to remove KCl and the filtrate is concentrated under reduced pressure to remove DMF and the product analyzed by GLC. The product is dissolved in ethyl acetate (300 mL) and extracted with 2N NaOH (2×100 mL) and water (100 mL). The organic phase is dried and concentrated to give pure methyl 2-(4-acetylphenoxy)propanoate (25 g) (yield 64%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05008439uspto-grants-1991_04