Example 147 Steps for the synthesis of 1-[4-(6-(methylamino)purin-9-yl)phenyl]-3-[3-(4-methylpiperazin-1-ylmethyl)-5-(trifluoromethyl)phenyl]urea (Table 2, compound 25):
Step A Preparation of 6-methylaminopurine
Dissolve 12.5 g (79 mmol) of 6-chloropurine in 20 mL of 40% methanol solution of methylamine and 20 mL of ethanol. The reaction solution was sealed in a reaction tube and stirred at 120 °C for 4 hours. After completion of the reaction, the reaction solution was concentrated, ground with water, filtered to collect the solid, washed with water and dried under vacuum to give 10.78 g (90% yield) of 6-methylaminopurine as a white solid.
1H-NMR (270 MHz, DMSO-d6) δ (ppm): 2.98 (3H, br.s), 7.58 (1H, br.s), 8.06 (1H, s), 8.19 (1H, br.s), 12.89 (1H, br.s).
ESI (LC-MS positive mode) m/z 150 (M + H).
