تفاعل #71012

معادلة التفاعل

4-hydroxybenzophenone

potassium carbonate

4-hydroxybutylacrylate glycidylether

→

yellow oil

المردود 101.1%

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

المردود 101.1%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated to reflux
2. 2
   درجة الحرارةat reflux temperature for 24 hours
3. 3
   ترشيحfiltered
4. 4
   أخرىto remove the undissolved potassium carbonate
5. 5
   أخرىThe filtrate was evaporated under reduced pressure
6. 6
   workup.ADDITIONThe residual oil was diluted with ethyl acetate (250 ml)
7. 7
   استخلاصextracted with a mixture of an aqueous solution of sodium hydroxide (1N)
8. 8
   workup.DISTILLATIONdistilled water (4/1)
9. 9
   أخرىThe organic layer was separated
10. 10
    تجفيفdried over MgSO4
11. 11
    ترشيحfiltered
12. 12
    أخرىevaporated

الإجراء التجريبي

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.

المصدر