반응 #217092

반응 방정식

NaOH

epichlorohydrin

epichlorohydrin

4-hydroxyphenyl benzyl ketone

NaOH

NaOH

→

4-Glycidyloxyphenyl benzyl ketone

용매

H2O

반응 조건

후처리

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

실험 절차

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.

출처