反应详情

温度

80 °C

A mixture of 2.2 g (6.5 mmol) of 2-methyl-4-methylsulfonyl-3-(4-methylthiophenyl)benzoic acid, 2.2 mL (19.6 mmol) of 30 percent hydrogen peroxide, and 25 mL of acetic acid was heated to 80° C. with stirring for 1 hour and was then allowed to stand overnight. The mixture was diluted with water, treated with sodium bisulfite, and then extracted with a mixture of ether and ethyl acetate. The extract was concentrated by evaporation under reduced pressure and the residue was diluted with dichloromethane. The resulting mixture was filtered and the solids that were collected were washed with ethyl acetate. The filtrate was found to contain only about 0.5 g of impure product and was discarded. The solids were dissolved (a slow process) in a mixture of ethyl acetate and water and the organic phase was separated and concentrated by evaporation under reduced pressure. The resulting solid residue was diluted with hexane and the insoluble solids were recovered by filtration and dried to obtain 2.1 g (88 percent of theory) of the title compound as a white powder melting at 214-215° C.

1. waitto stand overnight
2. extractionextracted with a mixture of ether and ethyl acetate
3. concentrationThe extract was concentrated by evaporation under reduced pressure
4. additionthe residue was diluted with dichloromethane
5. filtrationThe resulting mixture was filtered
6. customthe solids that were collected
7. washwere washed with ethyl acetate
8. dissolutionThe solids were dissolved (a slow process)
9. additionin a mixture of ethyl acetate and water
10. customthe organic phase was separated
11. concentrationconcentrated by evaporation under reduced pressure
12. additionThe resulting solid residue was diluted with hexane
13. filtrationthe insoluble solids were recovered by filtration
14. customdried