反应详情

温度

160 °C

A glass microwave reaction vessel was charged with 6-(4-chloropyridin-3-yl)-2-methylpyrimidin-4-amine (22 mg, 100 μmol), 1H-indazol-4-amine (27 mg, 199 μmol, Bionet) and EtOH (1 mL). The reaction mixture was stirred and heated in a Smith Synthesizer® microwave reactor (Personal Chemistry, Inc., Upssala, Sweden) at 160° C. for 30 min. The reaction mixture was diluted with saturated NaHCO3 (2 mL) and extracted with EtOAc (3×20 mL). The organic extract was washed with saturated NaCl (2 mL), dried over Na2SO4, filtered, concentrated and the residue was purified by silica gel chromatography, eluting with 10% MeOH/CH2Cl2/1% NH4OH to give N-(3-(6-amino-2-methylpyrimidin-4-yl)pyridin-4-yl)-1H-indazol-4-amine (14 mg, 44% yield). 1H NMR (300 MHz, CD3OD) δ 8.71 (s, 1H); 8.19 (d, J=6.14 Hz, 1H); 7.34-7.53 (m, 2H); 7.29 (d, J=7.02 Hz, 1H); 7.18 (d, J=6.28 Hz, 1H); 6.90 (s, 1H); 2.59 (s, 3H). m/z (ESI, +ve ion) 318 (M+H)+.

1. customA glass microwave reaction vessel
2. extractionextracted with EtOAc (3×20 mL)
3. extractionThe organic extract
4. washwas washed with saturated NaCl (2 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customthe residue was purified by silica gel chromatography
9. washeluting with 10% MeOH/CH2Cl2/1% NH4OH