反应详情

Bromine (0.18 mL, 3.5 mmol) was added to a solution of 2-(2-benzoylamino-4-pyridyl)-1-(4-methoxyphenyl)ethanone (1.2 g, 3.4 mmol) in acetic acid (10 mL) and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was concentrated. The residue was dissolved in N,N-dimethylformamide (20 mL), thioacetamide (0.30 g, 19 mmol) was added to the solution and the mixture was stirred at room temperature for 20 hours. An aqueous saturated solution of sodium hydrogencarbonate (20 mL) was added to the reaction mixture, the resulting mixture was extracted with ethyl acetate and the extract was washed with water. The extract was dried and concentrated. The residue was purified by silica gel column chromatography (hexane:ethyl acetate, 1:1) to obtain 0.68 g (yield 50%) of the title compound.

1. concentrationThe reaction mixture was concentrated
2. dissolutionThe residue was dissolved in N,N-dimethylformamide (20 mL)
3. stirringthe mixture was stirred at room temperature for 20 hours
4. extractionthe resulting mixture was extracted with ethyl acetate
5. washthe extract was washed with water
6. customThe extract was dried
7. concentrationconcentrated
8. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate, 1:1)