HRID1857209

反应详情

EQUATION

反应方程式

HRID 1857209 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To commercially available nitromethane (5 ml) were added commercially available anisole (0.5 ml), commercially available cyclohexanecarbonyl chloride (0.63 ml) and commercially available ytterbium(III) trifluoromethanesulfonate (288 mg), and the admixture was stirred at 60° C. for 3 hours. The reaction mixture was partitioned between water and chloroform, and the chloroform layer was washed with saturated aqueous sodium hydrogen carbonate and brine and then dried with anhydrous sodium sulfate. After removing the solvent by reduced-pressure distillation, the resulting residue was purified by chromatography on silica gel eluting with chloroform to obtain 517 mg of the title compound (yield: 51%).

WORKUP

后处理

  1. customThe reaction mixture was partitioned between water and chloroform
  2. washthe chloroform layer was washed with saturated aqueous sodium hydrogen carbonate and brine
  3. dry with materialdried with anhydrous sodium sulfate
  4. customAfter removing the solvent
  5. distillationby reduced-pressure distillation
  6. customthe resulting residue was purified by chromatography on silica gel eluting with chloroform