反应详情

A mixture of 140 mg of 5-[4-(4,6-dihydroxy-2,5,7,8-tetramethylchroman-2-ylmethoxy)benzyl]thiazolidine-2,4-dione (prepared as described in Example 30), 10 mg of p-toluenesulfonic acid, 10 ml of benzene and 0.5 ml of dimethylformamide was heated under reflux for 1 hour. The reaction solution was cooled, washed with a saturated aqueous solution of sodium bicarbonate and then with water and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography eluted with a 4:1 by volume mixture of benzene and ethyl acetate, to give the title compound, softening at 173°-176° C.

1. temperaturewas heated
2. temperatureunder reflux for 1 hour
3. temperatureThe reaction solution was cooled
4. washwashed with a saturated aqueous solution of sodium bicarbonate
5. dry with materialwith water and dried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was purified by silica gel column chromatography
8. washeluted with a 4:1 by volume mixture of benzene and ethyl acetate