反应详情

To a solution of 2-[1-(piperidin-3-yl)-ethylamino]-4-[benzimidazol-1-yl]pyrimidine (EXAMPLE 18) (20.9 mg, 0.065 mmol) in EtOH (0.6 mL) was added iodomethane (40 μL, 0.65 mmol). The mixture was placed in an oil bath at 60° C. and heated for 4 h, then stirred at room temperature overnight. The solvent was removed under reduced pressure, and the crude product was purified by preparative thin layer chromatography (1:9 2M NH3 in MeOH:CH2Cl2) to obtain 4.1 mg of the title compound. Partial 1H NMR (500 MHz, CDCl3): δ 8.61 (s, 1H); 8.35 (br s, 1H); 8.16 (d, J=7.5 Hz, 1H); 7.84 (d, J=7.1 Hz, 1H); 7.37 (m, 2H); 6.75 (d, J=5.5 Hz, 1H); 4.12 (m, 1H); 2.92 (d, J=9 Hz, 1H); 2.8 (d, J=11 Hz, 1H); 2.27 (s, 3H); 1.26 (d, J=6.7 Hz, 3H). Mass spectrum 337.3 (ESI, M+1).

1. customThe mixture was placed in an oil bath at 60° C.
2. temperatureheated for 4 h
3. customThe solvent was removed under reduced pressure
4. customthe crude product was purified by preparative thin layer chromatography (1:9 2M NH3 in MeOH:CH2Cl2)