HRID2304605
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 solution of N-methylthiourea (484 mg) in acetonitrile (40 mL), was added 2-bromo-2-phenyl-1-(3-pyridyl)ethanone hydrobromide (2.0 g), and then triethylamine (0.8 mL) was added dropwise to the mixture with stirring. After addition, the resulting mixture was stirred at reflux for 3 h and the solvent was evaporated. An aqueous saturated solution of sodium hydrogen carbonate was added to the residue and extracted with ethyl acetate. The extracts were washed with water, dried and the solvent was evaporated. The crystalline residue was recrystallized from ethyl acetate-isopropyl ether to give the title compound (1.2 g, yield 80%).
WORKUP
后处理
- additionAfter addition
- stirringthe resulting mixture was stirred
- temperatureat reflux for 3 h
- customthe solvent was evaporated
- additionAn aqueous saturated solution of sodium hydrogen carbonate was added to the residue
- extractionextracted with ethyl acetate
- washThe extracts were washed with water
- customdried
- customthe solvent was evaporated
- customThe crystalline residue was recrystallized from ethyl acetate-isopropyl ether