HRID12439

反应详情

EQUATION

反应方程式

HRID 12439 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Azido-5-chloro-2,4-dimethoxy-benzene (0.4 g, 1.9 mmol), 3-(4-Fluoro-phenyl)-3-oxo-propionic acid methyl ester (0.42 g, 2.2 mmol) and sodium ethoxide in EtOH (70 mg of sodium in 15 mL EtOH) were refluxed for 3 hours. During the reaction, the solution turned brown from dark green. After that, EtOH was evaporated off and the resulting oil was dried in vacuum. Trituration with ether (15 mL) gave light brown solids, which were removed by filtration and washed with ether. The solids then re-dissolved in CHCl3 and filtered. After evaporation of the solvent, light brown solids were obtained (0.35 g, 50%).

WORKUP

后处理

  1. customDuring the reaction
  2. customAfter that, EtOH was evaporated off
  3. customthe resulting oil was dried in vacuum
  4. customTrituration with ether (15 mL) gave light brown solids, which
  5. customwere removed by filtration
  6. washwashed with ether
  7. dissolutionThe solids then re-dissolved in CHCl3
  8. filtrationfiltered
  9. customAfter evaporation of the solvent
  10. customlight brown solids were obtained (0.35 g, 50%)