反应详情

To a suspension of thiourea (0.52 g) in acetonitrile (40 mL) was added 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide (2.5 g) and triethylamine (0.95 mL) was slowly added dropwise with stirring. After completion of dropwise addition, the mixture was stirred at a refluxing temperature for 3 h, and after allowing to cool, the precipitated crystals were collected by filtration. The crystals were washed successively with saturated sodium hydrogencarbonate solution, water, ethanol and ethyl ether and dried. The obtained crude crystals were recrystallized from tetrahydrofuran to give the title compound (1.5 g, yield 90%).

1. additionwas slowly added dropwise
2. additionAfter completion of dropwise addition
3. stirringthe mixture was stirred at a refluxing temperature for 3 h
4. temperatureto cool
5. filtrationthe precipitated crystals were collected by filtration
6. washThe crystals were washed successively with saturated sodium hydrogencarbonate solution, water, ethanol and ethyl ether
7. customdried
8. customThe obtained crude crystals
9. customwere recrystallized from tetrahydrofuran