反应详情

To a solution of 2-[1-(piperidin-3-yl)-ethylamino]-4-[benzimidazol-1-yl]pyrimidine (EXAMPLE 18) (51 mg, 0.16 mmol) in CH2Cl2 (1.6 mL) was added methylisocyanate (10.5 lL, 0.176 mmol) at room temperature. After the reaction was complete (2-3 h), the solvent was removed under reduced pressure, and the crude product was purified by preparative thin layer chromatography (4:1 acetone:hexane system as an eluent) to obtain the title compound. Partial 1H NMR (500 MHz, CDCl3): δ 8.61 (s, 1H); 8.36 (d, J=5.0 Hz, 1H); 8.16 (d, J=7.6 Hz, 1H); 7.85 (d, J=7.1 Hz, 1H); 7.38 (m, 2H); 6.78 (d, J=5.5 Hz, 1H); 4.17 (m, 1H); 4.07 (d, J=11 Hz, 1H); 3.76 (d, J=12.6 Hz, 1H); 2.78 (d, J=4.6 Hz, 3H); 1.31 (d, J=6.6 Hz, 3H). Mass spectrum 380.3 (ESI, M+1).

1. custom(2-3 h)
2. customthe solvent was removed under reduced pressure
3. customthe crude product was purified by preparative thin layer chromatography (4:1 acetone