反应详情

温度

70 °C

A 100 mL 3-neck flask was equipped with a magnetic stirrer, a reflux condenser, a nitrogen blanket, and a heating mantle with a temperature controller and a thermocouple. The flask was charged with o-phenylphenol (3.42 grams, 0.02 moles), with KOH pellets (1.37 grams, 0.02 moles, 85%), and with 15 mL of DMSO. The mixture was stirred at 100° C. under nitrogen until all of the KOH had dissolved (about 2 hours). The dark solution was cooled to 70° C., then the 1-chlorohexadecane (5.22 grams, 0.02 moles) was then added all at once. An exotherm to about 80° C. was observed. The reaction mixture was then stirred at 75° C. for about 7.5 hours, then it was poured into about 500 mL of water; solids separated. After stirring at room temperature for about 2 hours, the mixture was filtered. The solids were washed on the filter with a little water, then they were air dried to give 7.58 grams of waxy white solid. The yield was 96%; mp=35-37° C. Structure was confirmed by IR, GC/MS, and 1H- and 13C-NMR analyses.

1. customA 100 mL 3-neck flask was equipped with a magnetic stirrer, a reflux condenser
2. dissolutionhad dissolved (about 2 hours)
3. customto about 80° C.
4. customsolids separated
5. stirringAfter stirring at room temperature for about 2 hours
6. filtrationthe mixture was filtered
7. washThe solids were washed on the
8. filtrationfilter with a little water
9. customdried