反应详情

6(N,N-Dimethylamino)-pyrido[3,4-d]pyrimidin-4-one (12 g) was carefully treated with phosphorus oxychloride (42 ml) and triethylamine (18 ml) at room temperature under N2. After 1 hour at room temperature and 1 hour at 50° C., the mixture was concentrated in vacuo, azeotroping with toluene, then taken up in ethyl acetate, washed with sodium bicarbonate solution, dried and concentrated in vacuo to give the title compound (10.34 g); δH CDCl3 9.13(1H,s), 8.74(1H,s), 6.69(1H,s), 3.25(6H,s).

1. concentration1 hour at 50° C., the mixture was concentrated in vacuo
2. customazeotroping with toluene
3. washwashed with sodium bicarbonate solution
4. customdried
5. concentrationconcentrated in vacuo