反应详情

A solution of triethylamine (3.44 mL) in dehydrated dichloromethane was added to a mixture composed of 1-(2-amino-4,6-dichloropyrimidin-5-yl)-2-(2,2-dimethyl-[1,3]dioxolan-4-yl)ethan-1-one of 3) above (1.68 g), [(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-hydrazine hydrochloride of 4) above (2.87 g) and dehydrated dichloromethane (60 mL) under cooling in an ice bath over 20 minutes. The ice bath was removed, followed by stirring for two hours. Then, the reaction mixture was separated with chloroform and water. The organic layer was washed with water and then dried over anhydrous magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate-chloroform) to obtain the title compound (1.79 g, 75%) as a solid.

1. temperatureunder cooling in an ice bath over 20 minutes
2. customThe ice bath was removed
3. customThen, the reaction mixture was separated with chloroform and water
4. washThe organic layer was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationAfter filtration
7. concentrationthe filtrate was concentrated under reduced pressure
8. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate-chloroform)