反应详情

温度

65 °C

A mixture of 5-bromo-2-chloro-4-(prop-2-ynyloxy)pyrimidine (15 g), methyl 3,5-diaminobenzoate (45 g) and concentrated hydrochloric acid (15 ml) in methanol (600 ml) was stirred at 65° C. for 8 h. After concentration to half the volume water was added and the precipitate collected by filtration. The precipitate then was treated with sodium hydroxide solution (1 n) and dichloromethane. The organic phase then was washed with water and brine, dried (Na2SO4) and evaporated to dryness to give the title compound (13.8 g).

1. concentrationAfter concentration to half the volume water
2. additionwas added
3. filtrationthe precipitate collected by filtration
4. additionThe precipitate then was treated with sodium hydroxide solution (1 n) and dichloromethane
5. washThe organic phase then was washed with water and brine
6. dry with materialdried (Na2SO4)
7. customevaporated to dryness