反应详情

A mixture of 2,5-dimethoxytetrahydrofuran (39.6 g), o-aminophenol (36 g), dioxane (300 ml), and glacial acetic acid (180 ml) are heated under reflux for 4 hr. The solvents are removed and the residue distributed between ethyl acetate and 5% NaHCO3. The organic phase is washed with water, dried (MgSO4), filtered, and evaporated. The dark oily residue is subjected to chromatography on 2 kg of silica and eluted with chloroform to afford an oil. After being covered with hexane and stored for several days, the oil solidifies giving the title compound, m.p. 52° - 54° C. (Reported m.p. by Artico, et al., cited above, 45° - 47° C).

1. temperatureare heated
2. temperatureunder reflux for 4 hr
3. customThe solvents are removed
4. washThe organic phase is washed with water
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. washeluted with chloroform
9. customto afford an oil
10. waitstored for several days