Reaktion #71012

Reaktionsgleichung

4-hydroxybenzophenone

potassium carbonate

4-hydroxybutylacrylate glycidylether

→

yellow oil

Ausbeute 101.1%

acrylic acid 4-[3-(4-benzoyl-phenoxy)-2-hydroxy-propoxy]butyl ester

Ausbeute 101.1%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated to reflux
2. 2
   Temperaturat reflux temperature for 24 hours
3. 3
   Filtrationfiltered
4. 4
   Sonstigeto remove the undissolved potassium carbonate
5. 5
   SonstigeThe filtrate was evaporated under reduced pressure
6. 6
   workup.ADDITIONThe residual oil was diluted with ethyl acetate (250 ml)
7. 7
   Extraktionextracted with a mixture of an aqueous solution of sodium hydroxide (1N)
8. 8
   workup.DISTILLATIONdistilled water (4/1)
9. 9
   SonstigeThe organic layer was separated
10. 10
    Trocknendried over MgSO4
11. 11
    Filtrationfiltered
12. 12
    Sonstigeevaporated

Vorschrift

A reaction mixture containing 4-hydroxybenzophenone (14.9 g, 75 mmol), acetonitrile (40 mL), potassium carbonate (7.8 g, 56.25 mmol) and 4-hydroxybutylacrylate glycidylether (7.5 g, 37.5 mmol) was heated to reflux. The mixture was allowed to stir at reflux temperature for 24 hours. The mixture was cooled to room temperature and filtered to remove the undissolved potassium carbonate. The filtrate was evaporated under reduced pressure. The residual oil was diluted with ethyl acetate (250 ml) and extracted with a mixture of an aqueous solution of sodium hydroxide (1N) and distilled water (4/1). The organic layer was separated, dried over MgSO4, filtered and evaporated to provide 15.1 g of a yellow oil. The product was purified on a SVP D40 Merck Np Column using dichloromethane/n-hexane (50/50) as eluent, to afford 5.5 g of a yellow oil.

Quelle