反应详情

A mixture of N2-methyl-6-trifluoromethylpyridin-2,3-diamine (0.96 g), 2-ethylsulfanylbenzoic acid (1.01 g), WSC (1.06 g), and pyridine (5 ml) was stirred under reflux for 3 hours. Into the reaction mixture cooled to room temperature, water was poured, and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. To the resulting residue, a mixture of tripotassium phosphate (2.65 g) and 1-propanol (10 ml) was added, and stirred under reflux for 4 hours. Into the reaction mixture cooled to room temperature, water was poured, and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography to give 0.98 g of 2-(2-ethylsulfanylphenyl)-3-methyl-5-trifluoromethyl-3H-imidazo[4,5-b]pyridine (hereinafter referred to as Present Compound 151).

1. temperatureunder reflux for 3 hours
2. extractionextracted with ethyl acetate
3. dry with materialThe organic layer was dried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. additionTo the resulting residue, a mixture of tripotassium phosphate (2.65 g) and 1-propanol (10 ml)
6. additionwas added
7. stirringstirred
8. temperatureunder reflux for 4 hours
9. temperatureInto the reaction mixture cooled to room temperature
10. additionwater was poured
11. extractionextracted with ethyl acetate
12. dry with materialThe organic layer was dried over sodium sulfate
13. concentrationconcentrated under reduced pressure