反应详情

To a solution of 2-bromo-1-(3,5-dimethylphenyl)-2-(4-pyridyl)ethanone hydrobromide (5.0 g, 13 mmol) and thiourea (1.0 g, 14 mmol) in acetonitrile (60 mL) was added dropwise triethylamine (1.9 ml, 14 mmol) and the mixture was stirred at room temperature for 3 h. The solvent was concentrated under reduced pressure and a saturated aqueous sodium hydrogencarbonate solution was added to the residue. The mixture was extracted with ethyl acetate. The organic layer was washed with water and the solvent was evaporated. The obtained crude crystals were recrystallized from ethyl acetate to give the title compound (2.0 g, 7.2 mmol, yield 55%).

1. concentrationThe solvent was concentrated under reduced pressure
2. additiona saturated aqueous sodium hydrogencarbonate solution was added to the residue
3. extractionThe mixture was extracted with ethyl acetate
4. washThe organic layer was washed with water
5. customthe solvent was evaporated
6. customThe obtained crude crystals
7. customwere recrystallized from ethyl acetate