反应详情

温度

120 °C

4-fluoroaniline(0.46 ml, 4.70 mmol) and triethylamine(0.66 ml, 4.70 mmol) were added to a solution of 5,6-dimethyl-2-chloro-4-(1-methyl-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinolin-2-yl)pyrimidine(1.0 g, 3.13 mmol) in dimethyifomiamide(5 ml) and then stirred for 3 hours at 120° C. The reaction mixture was cooled to a room temperature and diluted with dichloromethane. Aqueous sodium hydroxide solution was added to the reaction mixture, which was then stirred. The dichloromethane layer was dried over anhydrous magnesium sulfate, concentrated under a reduced pressure. The resulting residue was purified by a silica gel column chromatography and dissolved in ethanol. Ethyl ether saturated with hydrochloric acid was added to the solution. The resulting solid was filtered and dried to give 530 mg of the titled compound.

1. temperatureThe reaction mixture was cooled to a room temperature
2. stirringwas then stirred
3. dry with materialThe dichloromethane layer was dried over anhydrous magnesium sulfate
4. concentrationconcentrated under a reduced pressure
5. customThe resulting residue was purified by a silica gel column chromatography
6. dissolutiondissolved in ethanol
7. additionEthyl ether saturated with hydrochloric acid was added to the solution
8. filtrationThe resulting solid was filtered
9. customdried