反应详情

温度

120 °C

Into a solution of N3-phenylbenzo[b]thiophene-2,3-diamine (16 g, 66.7 mmol) in trimethoxymethane (200 ml) was added formic acid (1.5 ml, 42.3 mmol) at room temperature. The reaction mixture was subsequently heated at 120° C. for 6 h. After cooling to room temperature, it was quenched with aqueous NaHCO3 solution and extracted with ethyl acetate. Upon evaporation off the solvent, the residue was purified by chromatography on silica gel with hexane/EtOAc (95/5, v/v) as eluent to yield 1-phenyl-1H-benzo[4,5]thieno[2,3-d]imidazole (9.0 g, 54%) as a solid.

1. temperatureAfter cooling to room temperature
2. customit was quenched with aqueous NaHCO3 solution
3. extractionextracted with ethyl acetate
4. customUpon evaporation off the solvent
5. customthe residue was purified by chromatography on silica gel with hexane/EtOAc (95/5