反应详情

A mixture of 1 g of 5-{4-[6-hydroxy-4-(E)-hydroxyimino-2,5,7,8tetramethylchroman-2-ylmethoxy ]benzyl}thiazolidine-2,4-dione (prepared as described in Example 13), 1.3 g of acetic anhydride and 10 ml of pyridine was allowed to stand for 8 days at room temperature, after which it was heated for 8 hours at 60°-80° C. An aqueous solution of potassium carbonate and ethyl acetate were then added to the reaction mixture. The organic layer was separated and dried over anhydrous sodium sulfate. The solvent was distilled off and the residue was purified by silica gel column chromatography, eluted with a 4:1 by volume mixture of hexane and ethyl acetate, to give the title compound, softening at 93°-97° C.

1. temperatureafter which it was heated for 8 hours at 60°-80° C
2. customThe organic layer was separated
3. dry with materialdried over anhydrous sodium sulfate
4. distillationThe solvent was distilled off
5. customthe residue was purified by silica gel column chromatography
6. washeluted with a 4:1 by volume mixture of hexane and ethyl acetate