反应详情

温度

95 °C

1-[(3-Amino-5,6-dimethyl-2-phenoxypyridin-4-yl)amino]eth-2-yl acetate (10.5 g, 33.29 mmol), toluene (100 mL), pyridine hydrochloride (0.077 g, 0.6659 mmol), and triethyl orthoacetate (9.1 mL, 49.94 mmol) were combined with stirring and the resulting mixture was heated to a gentle reflux (about 95° C.) for 1.5 hours. The reaction was complete. The resulting reaction mixture was concentrated under reduced pressure to white solids, which were dissolved in ethyl acetate. The ethyl acetate solution was washed with water (3×) and brine (2×), dried with magnesium sulfate, filtered, and concentrated under reduced pressure. The resulting solid was triturated with diethyl ether, filtered off, and dried at 60° C. overnight to provide 11.1 g of pure product, which was carried on to the next step.

1. temperaturethe resulting mixture was heated to
2. customThe resulting reaction mixture
3. concentrationwas concentrated under reduced pressure to white solids, which
4. dissolutionwere dissolved in ethyl acetate
5. washThe ethyl acetate solution was washed with water (3×) and brine (2×)
6. dry with materialdried with magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe resulting solid was triturated with diethyl ether
10. filtrationfiltered off
11. customdried at 60° C. overnight