反应详情

温度

140 °C

3-(2-chloroethoxy)-N-[3-chloro-4-(pyridin-2-ylmethoxy)phenyl]-1H-pyrazolo[3,4-d]pyrimidin-4-amine (prepared as described in Example 13/200 mg, 0.43 mmol), pyrrolidine (178 μL, 2.14 mmol) and potassium iodide (0.43 mmol) were mixed in DMA (2 ml). The mixture was heated at 140° C. for 3 minutes in a microwave reactor. The crude mixture was then filtered and purified by preparative HPLC (column beta-basic, Hypercil 51 μm, 21×100 mm) eluting with a mixture of water and acetonitrile containing 2g/l of ammonium carbonate (gradient). After evaporation of the solvents, the remaining solid was triturated in ether, filtered and dried to give the title compound (101 mg, 51%); NMR Spectrum: 1.66 (br s, 4H), 2.54 (br s, 4H), 2.88 (t, 2H), 4.42 (t, 2H), 5.29 (s, 2H), 7.24 (d, 1H), 7.37 (t, 1H), 7.55-7.58 (m, 2H), 7.86-7.90 (m, 2H), 8.29 (s, 1H), 8.60 (br s, 2H); Mass Spectrum: 466 (MH+).

1. filtrationThe crude mixture was then filtered
2. custompurified by preparative HPLC (column beta-basic, Hypercil 51 μm, 21×100 mm)
3. washeluting with a mixture of water and acetonitrile containing 2g/l of ammonium carbonate (gradient)
4. customAfter evaporation of the solvents
5. customthe remaining solid was triturated in ether
6. filtrationfiltered
7. customdried