反应详情

To a solution of 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine (1 g, 3.89 mmol) in DMF (30 mL) is added 2-bromobenzaldehyde (0.7 mL, 5.83 mmol) at room temperature. Oxone (2.4 g, 3.89 mmol) in H2O (5 mL) is added and the solution is stirred for 1 hour. Saturated sodium thiosulfate solution (10 mL) is added and the mixture is extracted with EtOAc (3×15 mL) and H2O (20 mL). The combined organic layer is dried (MgSO4), filtered and concentrated. The residue is purified by silica gel flash column chromatography eluting with 10% MeOH in CH2Cl2 to afford 5-[2-(2-bromo-phenyl)-1-tert-butyl-1H-benzimidazol-5-yl]-pyrimidin-2-ylamine (800 mg, 48%) as a white solid.

1. extractionthe mixture is extracted with EtOAc (3×15 mL) and H2O (20 mL)
2. dry with materialThe combined organic layer is dried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue is purified by silica gel flash column chromatography
6. washeluting with 10% MeOH in CH2Cl2