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 2-chloro-5-nitropyridine (25 g) and 2-(5-methyl-2-phenyl-4-oxazolyl)ethanol (32.1 g) in THF (250 ml) was added, in small portions, sodium hydride (60% in oil, 6.92 g), and the mixture was stirred. The reaction mixture was stirred, at room temperature, for further 15 hours, which was poured into water, followed by extraction with ethyl acetate. The ethyl acetate layer was washed with water and dried (MgSO4), then the solvent was distilled off under reduced pressure. The residual crystals are collected by filtration, followed by recrystallization from ethanol to afford 2-[2-(5-methyl-2-phenyl-4-oxazolyl)ethoxy]-5-nitropyridine (25.4 g, 49%) as yellowish brown crystals, m.p.110.5°-111.5° C.
WORKUP
后处理
- stirringThe reaction mixture was stirred, at room temperature, for further 15 hours
- extractionfollowed by extraction with ethyl acetate
- washThe ethyl acetate layer was washed with water
- dry with materialdried (MgSO4)
- distillationthe solvent was distilled off under reduced pressure
- filtrationThe residual crystals are collected by filtration
- customfollowed by recrystallization from ethanol