反应详情

Into a flask were charged 80.7 mg (0.29 mmol) of 4-nonanoyloxy benzoic acid, 84.2 mg (0.27 mmol) of 4-hydroxy-4'-(2-methyloctanoyl) biphenyl, 63.5 mg (0.31 mmol) of dicyclohexylcarbodiimide, 6.0 mg (0.05 mmol) of 4-dimethylamino pyridine and 5 ml of dried dichloromethane, which was heated under reflux for 6 hours. After the cooling, the resulting solid was filtered off, and washed with dichloromethane. The organic phase was washed with 0.1 normal hydrochloric acid and then water, dried on anhydrous magnesium sulfate, and the solvent was distilled off. This product was purified by a column chromatography and recrystallized with ethanol to obtain 65.3 mg (yield 42%) of white 4-nonanoyloxy benzoic acid-4-(2-methyloctanoyl) biphenyl.

1. temperaturewas heated
2. temperatureunder reflux for 6 hours
3. filtrationAfter the cooling, the resulting solid was filtered off
4. washwashed with dichloromethane
5. washThe organic phase was washed with 0.1 normal hydrochloric acid
6. dry with materialwater, dried on anhydrous magnesium sulfate
7. distillationthe solvent was distilled off
8. customThis product was purified by a column chromatography
9. customrecrystallized with ethanol