反应详情

To a solution of 4-benzyloxy-phenylamine (2 g, 8.4 mmol) in 30 mL of DCM was added triethylamine (1 mL) and di-2-pyridylthionocarbonate (2.5 g, 8.4 mmol). The resulting mixture was stirred at RT for 2 h. The reaction mixture was diluted with DCM and washed with water and brine. The organic layer was then dried over Na2SO4, filtered and concentrated. The residue was dissolved in 30 mL DMF, N-methyl-benzene-1,2-diamine (1.5 g, 12.7 mmol) and EDCI (2 g, 10.5 mmol). The resulting mixture was heated at 70° C. for 4 h. The reaction was cooled to RT, diluted with ethyl acetate and washed with water and brine. Purification by silica gel chromatography (98:2 chlorforma/MeOH) afforded the desired product (4-benzyloxy-phenyl)-(1-methyl-1H-benzoimidazol-2-yl)-amine. [M+1]=330.1

1. washwashed with water and brine
2. dry with materialThe organic layer was then dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in 30 mL DMF
6. temperatureThe resulting mixture was heated at 70° C. for 4 h
7. temperatureThe reaction was cooled to RT
8. washwashed with water and brine
9. customPurification by silica gel chromatography (98:2 chlorforma/MeOH)