反应详情

温度

100 °C

To a solution of the title D compound of Example 1, 2-{5-amino-2-(furan-2-yl)-7H-pyrrolo[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-7-yl}ethyl methanesulfonate (0.06 g, 0.165 mmol) in dry DMF (5 mL), 2,4-difluorophenol (0.33 mmol) and 0.06 mL of DIEA are added, and the solution is stirred at 100° C. for 5 h. The reaction mixture is cooled to RT, and the solvent is removed under reduced pressure. To the residue, acetonitrile is added and the solution is stirred at 60° C. for 0.5 h. The solution is then cooled to RT, and the resulting solids are collected by filtration to give 7-(2-(2,4-difluorophenoxy)ethyl)-2-(furan-2-yl)-7H-pyrrolo[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5-amine: LC/MS (M+1=397.1). 1H NMR (DM50-d6, 400 MHz) δ 4.41 (m, 2H), 4.53 (m, 2H), 6.63 (m, 1H), 6.72 (m, 1H), 6.99 (m, 1H), 7.23 (m, 4H), 7.55 (br s, 2H, NH2), 7.92 (s, 1H). Anal. calculated for (C19H14F2N6O2+0.5 H2O): C, 56.30; H, 3.73; F, 9.37; N, 20.73; O, 9.87. Found C, 56.36; H, 3.59; N, 18.51.

1. temperatureThe reaction mixture is cooled to RT
2. customthe solvent is removed under reduced pressure
3. additionTo the residue, acetonitrile is added
4. stirringthe solution is stirred at 60° C. for 0.5 h
5. temperatureThe solution is then cooled to RT
6. filtrationthe resulting solids are collected by filtration