Reaktion #217092

Reaktionsgleichung

NaOH

epichlorohydrin

epichlorohydrin

4-hydroxyphenyl benzyl ketone

NaOH

NaOH

→

4-Glycidyloxyphenyl benzyl ketone

Lösungsmittel

H2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA 100 ml 3-neck round-bottom flask equipped with a magnetic stir bar
2. 2
   Temperaturthermometer and reflux condenser
3. 3
   workup.ADDITION~0.2 g per addition
4. 4
   Sonstigethe reaction temperature below 100° C
5. 5
   Sonstigewas removed by vacuum distillation with the flask temperature
6. 6
   Sonstigekept below 150° C
7. 7
   SonstigeThe residue was air-dried
8. 8
   Sonstigerecrystallized twice from ethanol
9. 9
   Sonstigeredried
10. 10
    SonstigeA 1H-NMR spectrum of this compound, with peak assignments, is provided in FIG. 1

Vorschrift

A 100 ml 3-neck round-bottom flask equipped with a magnetic stir bar, thermometer and reflux condenser was charged with 11.0 g epichlorohydrin, 5.0 g 4-hydroxyphenyl benzyl ketone, and 0.1 ml H2O. The reactants were stirred on a hotplate. NaOH was then added, ~0.2 g per addition, up to a total of 0.95 g NaOH. The rate of NaOH addition was controlled to keep the reaction temperature below 100° C. At the end of the exothermic reaction, excess epichlorohydrin was removed by vacuum distillation with the flask temperature kept below 150° C. The residue was air-dried, then recrystallized twice from ethanol and redried. The yield was 2.8 g (44%), m.p. 81.0°-82.4° C. A 1H-NMR spectrum of this compound, with peak assignments, is provided in FIG. 1.

Quelle