反应详情

温度

0 °C

A mixture of 6-(2-phenylethynyl)-4-(pyridin-4-yl)-5-(pyrimidin-5-yl)pyridin-2-amine G9 (72 mg, 0.21 mmol), DMAP (0.05 mg, 4 μmol) and Et3N (43 μl, 0.31 mmol) in dioxane (4.3 ml) is stirred at 0° C. for 15 minutes. 2-bromo-propionyl bromide (33 μl, 0.31 mmol) is added dropwise and the mixture stirred at RT for 1 h. The mixture is heated to 90° C. and stirred for 16 h. Et3N (43 μl, 0.31 mmol) and 2-Bromo-propionyl bromide (33 μl, 0.31 mmol) is added and the mixture stirred for another 3 h. The mixture is cooled to RT, methylamine (2 mol/l solution in THF, 1.03 ml, 2.06 mmol) is added and the mixture stirred for 17 h. The mixture is concentrated in vacuo and the product purified by RP HPLC. Yield: 7.6 mg (9%). HPLC-MS: M+H=435; tR=.2.75 min (METHOD—6).

1. stirringthe mixture stirred at RT for 1 h
2. temperatureThe mixture is heated to 90° C.
3. stirringstirred for 16 h
4. stirringthe mixture stirred for another 3 h
5. temperatureThe mixture is cooled to RT
6. stirringthe mixture stirred for 17 h
7. concentrationThe mixture is concentrated in vacuo
8. customthe product purified by RP HPLC
9. custom2.75 min (METHOD—6)