HRID233272

反应详情

EQUATION

反应方程式

HRID 233272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringThe reaction mixture was stirred, at room temperature, for further 15 hours
  2. extractionfollowed by extraction with ethyl acetate
  3. washThe ethyl acetate layer was washed with water
  4. dry with materialdried (MgSO4)
  5. distillationthe solvent was distilled off under reduced pressure
  6. filtrationThe residual crystals are collected by filtration
  7. customfollowed by recrystallization from ethanol