反应详情

温度

110 °C

To solid 2-(cis-2,6-dimethylmorpholino)-5-(2-methylpyridin-4-yl)pyrimidin-4-ol (8.3 g, 27.6 mmol) at 20° C. was added neat phosphorus oxychloride (79 ml, 848 mmol). The reaction mixture was stirred at 110° C. for 3 hours. After cooling to 30° C., most of the phosphorus oxychloride was removed and 20 ml of dichloromethane was added. The solution was added into ice-water. The pH was adjusted to 8 using sodium bicarbonate. The dichloromethane layer was separated, washed with water, dried and evaporated. The crude product was added to a silica gel column and was eluted with dichloromethane and then dichloromethane/methanol (5:1). Collected fractions were evaporated to give the title compound (680 mg, 1.960 mmol, 7.09% yield). LC/MS [M+H]+=319/321.

1. customwas removed
2. addition20 ml of dichloromethane was added
3. additionThe solution was added into ice-water
4. customThe dichloromethane layer was separated
5. washwashed with water
6. customdried
7. customevaporated
8. additionThe crude product was added to a silica gel column
9. washwas eluted with dichloromethane
10. customCollected fractions were evaporated