反应详情

A solution of p-bromophenol (138 g, 0.8 mole), cinnamic acid (148 g, 1.0 mole), acetic acid (200 g) and conc. sulfuric acid was refluxed for 2 h. Volatile material was distilled at reduced pressure. The residual syrup was cooled and triturated with cold water, giving a semi-crystalline mass. This was washed extensively with water, saturated sodium carbonate and finally with water again. The material was filtered through a sintered glass funnel, and then mixed with an equal weight of ethanol. The slurry was stirred at room temperature for 1 h and then filtered. The resulting product was washed briefly with ethanol and then diisopropyl ether. After drying, 135 g (55.7%) of the title compound was isolated as white crystals, melting at 117° C.

1. distillationVolatile material was distilled at reduced pressure
2. temperatureThe residual syrup was cooled
3. customtriturated with cold water
4. customgiving a semi-crystalline mass
5. washThis was washed extensively with water, saturated sodium carbonate and finally with water again
6. filtrationThe material was filtered through a sintered glass funnel
7. additionmixed with an equal weight of ethanol
8. filtrationfiltered
9. washThe resulting product was washed briefly with ethanol
10. customAfter drying