반응 #1172511

ord-ac68934f827e481a9fb094951a877288

반응 조건

온도
87.5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The reaction is filtered
  2. 2
    기타to remove KCl
  3. 3
    농축the filtrate is concentrated under reduced pressure
  4. 4
    기타to remove DMF
  5. 5
    workup.DISSOLUTIONThe product is dissolved in ethyl acetate (300 mL)
  6. 6
    추출extracted with 2N NaOH (2×100 mL) and water (100 mL)
  7. 7
    기타The organic phase is dried
  8. 8
    농축concentrated

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05008439uspto-grants-1991_04