反应详情

温度

50 °C

The compound (165 mg) produced in Example 55 was dissolved in DMSO (2 mL), a Wittig reagent (carboisopropoxymethylenetriphenylphosphorane, 218 mg) and 1-hydroxy-1,2-benziodoxol-3(1H)-one 1-oxide (IBX, 168 mg) were added, followed by stirring at 50° C. for 5 hours. Ethyl acetate and water were added to the reaction mixture, and insolubles were filtered. Extraction with ethyl acetate, and washing with an aqueous saturated sodium bicarbonate solution and a saline, and drying with anhydrous magnesium sulfate were carried out, followed by concentration under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=97:3→80:20) to obtain a titled compound (174 mg) having the following physical property values.

1. filtrationwere filtered
2. extractionExtraction with ethyl acetate
3. washwashing with an aqueous saturated sodium bicarbonate solution
4. dry with materiala saline, and drying with anhydrous magnesium sulfate
5. concentrationfollowed by concentration under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=97:3→80:20)