反应详情

温度

25 °C

To a 250 mL round-bottomed flask was added 6-bromo-1H-benzo[d]imidazol-2-amine (2.00 g, 9.43 mmol, Carbocore, The Woodlands, Tex.), DCM (100 mL), pyridine (1.0 mL, 12.3 mmol) and acetic anhydride (0.979 mL, 10.4 mmol). The mixture was stirred at 25° C. for 18 h. The solution was concentrated and then diluted with 10% MeOH (2M in NH3)/CH2Cl2 until homogeneous and then the solution was concentrated onto silica. Purification by silica gel chromatography (0.5 to 5.0% MeOH (2 M in NH3)/CH2Cl2) afforded the title compound as a white solid (0.676 g, 28%). MS (ESI, positive ion) m/z: 254 (M(79Br)+1).

1. concentrationThe solution was concentrated
2. additiondiluted with 10% MeOH (2M in NH3)/CH2Cl2 until homogeneous and then the solution
3. concentrationwas concentrated onto silica
4. customPurification by silica gel chromatography (0.5 to 5.0% MeOH (2 M in NH3)/CH2Cl2)