反应详情

A mixture of 50 g (0.238 mole) of ethyl homovanillate, 75 g (0.476 mole) of 1-bromo-3-chloropropane and 98.7 g (0.71 mole) of anhydrous potassium carbonate in 1 liter of acetone was heated at reflux for 24 hr. The mixture was filtered and the filtrate was concentrated under reduced pressure to give an oil which gradually crystallized to a semi-solid. The solid was recrystallized from ethyl ether-petroleum ether (30°-60° C.) to yield 44.4 g (65%) of white solid, m.p. 36°-38° C.

1. temperaturewas heated
2. temperatureat reflux for 24 hr
3. filtrationThe mixture was filtered
4. concentrationthe filtrate was concentrated under reduced pressure
5. customto give an oil which
6. customgradually crystallized to a semi-solid
7. customThe solid was recrystallized from ethyl ether-petroleum ether (30°-60° C.)