反应详情

温度

120 °C

A mixture of 0.40 g of N2-methyl-5-trifluoromethylpyridine-2,3-diamine, 0.41 g of 3-ethylisonicotinic acid, 0.44 g of WSC and 10 ml of pyridine was stirred for 2.5 hours at 120° C. The reaction mixture was cooled down to room temperature. Into the reaction mixture was poured water, and the mixture was extracted three times with ethyl acetate. The organic layer was dried over magnesium sulfate, then, concentrated under reduced pressure. To the residue was added a mixture of 0.60 g of p-toluenesulfonic acid monohydrate and 10 ml of toluene, and the mixture was stirred for 7 hours at 120° C. The reaction mixture was cooled down to room temperature. Into the reaction mixture was poured water, and the mixture was extracted three times with ethyl acetate. The organic layer was dried over magnesium sulfate, then, concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.10 g of 2-(3-ethylpyridin-4-yl-)-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine (hereinafter, referred to as present active compound 217).

1. temperatureThe reaction mixture was cooled down to room temperature
2. extractionthe mixture was extracted three times with ethyl acetate
3. dry with materialThe organic layer was dried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. additionTo the residue was added
6. additiona mixture of 0.60 g of p-toluenesulfonic acid monohydrate and 10 ml of toluene
7. stirringthe mixture was stirred for 7 hours at 120° C
8. temperatureThe reaction mixture was cooled down to room temperature
9. additionInto the reaction mixture was poured water
10. extractionthe mixture was extracted three times with ethyl acetate
11. dry with materialThe organic layer was dried over magnesium sulfate
12. concentrationconcentrated under reduced pressure