反应详情

温度

160 °C

A mixture of 4-aminoquinazoline (11.6 g) and diethyl ethoxymethylenepropanedioate (19.0 g) in N,N-dimethylformamide (40 ml) was stirred for 1 hour and 20 minutes at 160° C. and then cooled to 0° C. to precipirate crystals. To the mixture was added small volume of water with stirring. The crystals were separated by filtration, washed with water, dried overnight under reduced pressure and dissolved in ethyl acetate. The resultant solution was dried over anhydrous magnesium sulfate and recrystallized from a mixture of ethyl acetate and hexane to give crystalline diethyl [(4-quinazolinylamino)methylene]propanedioate (22.7 g).

1. temperaturecooled to 0° C.
2. stirringwith stirring
3. customThe crystals were separated by filtration
4. washwashed with water
5. customdried overnight under reduced pressure
6. dissolutiondissolved in ethyl acetate
7. dry with materialThe resultant solution was dried over anhydrous magnesium sulfate
8. customrecrystallized from a mixture of ethyl acetate and hexane