HRID499331

反应详情

EQUATION

反应方程式

HRID 499331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

tert-Butyl 3-(1-oxido-2-pyridyl)propanoate (0.88 g, 3.9 mmol) was dissolved in nitroethane (5 ml). Trimethylsilyl cyanide (0.78 g, 7.9 mmol) and N,N-dimethylcarbamoyl chloride (0.85 g, 7.9 mmol) were added thereto. The reaction mixture was stirred at room temperature for 48 hrs, combined with ethyl acetate and water. The organic layer was washed successively with saturated aqueous sodium hydrogen carbonate solution and saturated brine and dried over an hydrous magnesium sulfate. The solvent was evaporated. The residue was subjected to a silica gel (50 g) column chromatography and eluted with hexane-ethyl acetate (3:1, v/v) to give the titled compound (0.75 g, 82%).

WORKUP

后处理

  1. washThe organic layer was washed successively with saturated aqueous sodium hydrogen carbonate solution and saturated brine
  2. dry with materialdried over an hydrous magnesium sulfate
  3. customThe solvent was evaporated
  4. washeluted with hexane-ethyl acetate (3:1