反应详情

温度

80 °C

A mixture of N2-methyl-5-trifluoromethylpyridin-2,3-diamine (1.34 g), 2-methylsulfanylbenzaldehyde (1.28 g), sodium hydrogen sulfite (2.19 g), and DMF (14 ml) was stirred with heating at 80° C. for 1 hour, and then heated to 120° C., and stirred with heating for further 3 hours. Into the reaction mixture cooled to room temperature, saturated aqueous ammonium chloride solution was poured, and extracted with ethyl acetate 3 times. The combined organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography to give 0.74 g of 3-methyl-2-(2-methylsulfanylphenyl)-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine (hereinafter referred to as Present Compound 1).

1. temperatureheated to 120° C.
2. stirringstirred
3. temperaturewith heating for further 3 hours
4. temperatureInto the reaction mixture cooled to room temperature
5. extractionextracted with ethyl acetate 3 times
6. dry with materialThe combined organic layer was dried over magnesium sulfate
7. concentrationconcentrated under reduced pressure