HRID1062617
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a suspension of N-methylthiourea (0.24 g) in acetonitrile (18 mL) was added 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide (1.0 g) and triethylamine (0.4 mL) was slowly added dropwise with stirring. After completion of dropwise addition, the mixture was stirred at a refluxing temperature for 3 h, and the solvent was evaporated. To the residue was added saturated aqueous sodium hydrogencarbonate and the mixture was extracted with ethyl acetate, and the extract was washed with water and dried, and the solvent was evaporated. The remaining crude crystals were recrystallized from ethyl acetate-isopropyl ether to give the title compound (0.65 g, yield 85%).
WORKUP
后处理
- additionwas slowly added dropwise
- additionAfter completion of dropwise addition
- stirringthe mixture was stirred at a refluxing temperature for 3 h
- customthe solvent was evaporated
- additionTo the residue was added saturated aqueous sodium hydrogencarbonate
- extractionthe mixture was extracted with ethyl acetate
- washthe extract was washed with water
- customdried
- customthe solvent was evaporated
- customThe remaining crude crystals were recrystallized from ethyl acetate-isopropyl ether