反应详情

Bromine (0.11 mL, 2.1 mmol) was added to a solution of 2-(2-benzoylamino-4-pyridyl)-1-(4-methoxyphenyl)ethanone (0.72 g, 2.1 mmol) in acetic acid (20 mL) at 0° C. and the mixture was stirred at room temperature for 1 hour. The reaction mixture was concentrated. The residue was dissolved in acetonitrile. (20 mL), to the solution were added thiourea (0.17 g, 2.2 mmol) and triethylamine (0.35 mL, 2.5 mmol) and the mixture was stirred at 80° C. for 5 hours. After the reaction mixture was cooled to room temperature, a saturated aqueous solution of sodium hydrogencarbonate (200 mL) was added and the resulting solid was filtered and washed with water. The resulting crude crystals were collected by filtration and washed with water. The crude crystals were recrystallized from ethanol to obtain 0.17 g (0.43 mmol, yield 21%) of the title compound.

1. concentrationThe reaction mixture was concentrated
2. dissolutionThe residue was dissolved in acetonitrile
3. stirringthe mixture was stirred at 80° C. for 5 hours
4. temperatureAfter the reaction mixture was cooled to room temperature
5. filtrationthe resulting solid was filtered
6. washwashed with water
7. filtrationThe resulting crude crystals were collected by filtration
8. washwashed with water
9. customThe crude crystals were recrystallized from ethanol