反应详情

温度

180 °C

(4-Benzyloxy-phenyl)-(6-cyanoquinazolin-4-yl)-amine (0.106 g) in dimethylformamide was treated with sodium azide (0.06 g) and ammonium chloride (0.05 g) and the mixture stirred at 180° C. for 18 hours. The mixture was cooled, poured onto water and extracted with ethyl acetate/THF (3:1). The organic extracts were dried and concentrated in vacuo. The residue was purified using solid phase extraction to yield the title compound (0.024 g); δH [2H6]DMSO 10.18(1H,s), 9.25(1H,s), 8.55(1H,s), 8.40(1H,d), 7.88(1H,d), 7.74(2H,d), 7.45(6H,m), 7.07(2H,d), 5.17(1H,s), m/z (M+1)+396.

1. temperatureThe mixture was cooled
2. additionpoured onto water
3. extractionextracted with ethyl acetate/THF (3:1)
4. customThe organic extracts were dried
5. concentrationconcentrated in vacuo
6. customThe residue was purified
7. extractionsolid phase extraction