反应详情

A mixture of 2-(2-ethylsulfanylphenyl)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine (0.25 g), sodium periodate (0.24 g), methanol (6 ml), water (2 ml), and THF (0.8 ml) was stirred at room temperature for 20 minutes, and then heated to 50° C., and stirred with heating for further 1.5 hours. To the ice-cooled reaction mixture, water was added. The precipitated crystal was collected by filtration. The obtained crystal was dissolved in ethyl acetate, and washed with saturated aqueous sodium thiosulfate solution, saturated aqueous sodium hydrogen carbonate solution, then saturated brine, sequentially. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue was washed with hexane to give 0.20 g of 2-(2-ethylsulfinylphenyl)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine (hereinafter referred to as Present Compound 5).

1. temperatureheated to 50° C.
2. stirringstirred
3. temperaturewith heating for further 1.5 hours
4. additionwas added
5. filtrationThe precipitated crystal was collected by filtration
6. dissolutionThe obtained crystal was dissolved in ethyl acetate
7. washwashed with saturated aqueous sodium thiosulfate solution, saturated aqueous sodium hydrogen carbonate solution
8. dry with materialThe organic layer was dried over magnesium sulfate
9. concentrationconcentrated under reduced pressure
10. washThe resulting residue was washed with hexane