反应详情

温度

0 °C

A solution of 3-chloroperbenzoic acid (2.45 g, 0.0142 mol) in dichloromethane (40 ml) is added to a pre-cooled solution (0° C.) of 4-(4-bromo-2-ethylphenyl)-2,2,6,6-tetramethyl-thiopyran-3,5-dione (3.5 g, 0.0095 mol) in dichloromethane (100 ml). The reaction mixture is stirred at 0° C. for one hour and then allowed to come to room temperature. The reaction mixture is stirred at room temperature for one hour, diluted with water (100 ml) and separated. The organic phase is collected, and the aqueous layer is extracted with dichloromethane (2×50 ml). The organic phases are combined, washed with water, and dried over anhydrous sodium sulfate. The mixture is filtered, and the filtrate is evaporated under reduced pressure. The residue is purified by column chromatography on silica gel to give 4-(4-bromo-2-ethylphenyl)-2,2,6,6-tetramethyl-1-oxo-dihydrothiopyran-3,5-dione as a white solid (2.0 g).

1. customto come to room temperature
2. stirringThe reaction mixture is stirred at room temperature for one hour
3. customseparated
4. customThe organic phase is collected
5. extractionthe aqueous layer is extracted with dichloromethane (2×50 ml)
6. washwashed with water
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationThe mixture is filtered
9. customthe filtrate is evaporated under reduced pressure
10. customThe residue is purified by column chromatography on silica gel