反应详情

To a cold (0° C.) solution of (4-aminomethyl-benzyl)-(1H-benzimidazol-2-ylmethyl)-(5,6,7,8-tetrahydro-quinolin-8-yl)-amine (0.130 g, 0.33 mmol) in CH2Cl2 (3.5 mL) was added benzyl isocyanate (45 μL, 0.36 mmol) and the resultant solution was stirred for 100 minutes. The cooling bath was removed and the mixture was concentrated under reduced pressure. Purification of the crude material by column chromatography on silica gel (25:1:1 CH2Cl2—CH3OH—NH4OH) followed by radial chromatography on silica gel (1 mm plate, 25:1:1 CH2Cl2—CH3OH—NH4OH) provided the free base of the title compound (0.047 g, 28%) as a white solid.

1. customThe cooling bath was removed
2. concentrationthe mixture was concentrated under reduced pressure
3. customPurification of the crude material by column chromatography on silica gel (25:1:1 CH2Cl2—CH3OH—NH4OH)