反应详情

A solution of 41.5 g (0.3 mole) of 2-ethoxyphenol, 29.6 g (0.4 mole) of glycidol, 2 ml of pyridine and 150 ml of absolute ethanol was heated at reflux temperature for 18 hr. The mixture was concentrated to a thick oil that crystallized slowly over several days. The crude product was chromatographed on a silica gel column (1.2 kg) using increasing portions of acetone in methylene chloride to elute the product. The desired fractions were combined and concentrated to give a yellow oil that crystallized on standing. The solid was triturated with petroleum ether and the mixture filtered to obtain 41.8 g of solid. Recrystallization from carbon tetrachloride yielded 37.2 g (58%) of white solid, mp 64°-65° C.

1. temperatureat reflux temperature for 18 hr
2. concentrationThe mixture was concentrated to a thick oil that
3. customcrystallized slowly over several days
4. customThe crude product was chromatographed on a silica gel column (1.2 kg)
5. temperatureusing increasing portions of acetone in methylene chloride
6. washto elute the product
7. concentrationconcentrated
8. customto give a yellow oil that
9. customcrystallized
10. customThe solid was triturated with petroleum ether
11. filtrationthe mixture filtered